A method for producing concentrated whey protein nanogel, the obtained whey protein nanogel or nanogel composition, and a food containing such whey protein nanogel or nanogel composition.

Abstract

The present invention relates to the denaturation of whey proteins to produce special whey protein nanogels, and further to the resulting whey protein nanogels and their use in food products such as beverages. The whey protein nanogels provide very low viscosity contribution when used at high concentrations in beverages and liquid products, which demonstrates their uniqueness.

Description

[Technical Field]

[0001] This invention relates to the production of special whey protein nanogels by denaturing whey protein, and further to the use of the obtained whey protein nanogels and their use in food products such as beverages. When used in high concentrations in beverages and liquid products, these whey protein nanogels provide a very low viscosity contribution, which demonstrates their uniqueness. [Background technology]

[0002] The formation of micro or nanoparticles of denatured whey proteins has been previously described and is known as a method for modifying the functionality of whey proteins.

[0003] US 6,605,311 B2 discloses insoluble, denatured, heat-stable protein particles having an average diameter of 0.1–3 microns when hydrated, which are dispersible in aqueous solutions and are used in food and beverage products.

[0004] WO2007 / 110421 A2 discloses the preparation of nano-sized whey protein micelles by thermal denaturation of whey protein. Example 11 describes the formation of a whey protein micelle concentrate having a protein content of 20% w / w. The concentrate is described on page 28, section 2 of WO2007 / 110421A2 as having a "creamy semi-solid texture," which clearly indicates high viscosity.

[0005] CN105542195A discloses nanogels formed by the conjugation of polysaccharides and whey proteins and subsequent heat treatment, and further discloses the use of these nanogels in food. [Overview of the Initiative]

[0006] The inventors have discovered that special process conditions make it possible to produce nanogels of denatured whey protein in solution that have remarkably high concentrations of protein, particularly remarkably high concentrations of natural β-lactoglobulin (BLG), the main protein in whey and the driving force behind the thermal aggregation of whey protein. The ability to form nanogels at high protein concentrations is highly advantageous because it reduces energy consumption per kg of protein during processing, meaning that less solution must be heated and then cooled per kg of protein. This further reduces the cost of transporting the nanogel product in liquid form, because less water needs to be transported. It also reduces the cost of converting the nanogel suspension into powder, because less water needs to be removed.

[0007] Therefore, one aspect of the invention relates to a method for producing a whey protein nanogel composition, the method comprising: a) To provide a whey protein solution having the following: - A natural BLG content of at least 3% w / w, pH in the range of -5.8 to 7.5, preferably 5.8 to 6.5. - The weight ratio between the total amount of calcium and natural BLG is at most 0.010, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 25 mM, -If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 20 mM, b) Heat the whey protein solution to a temperature of at least 68°C for a period of time sufficient to form a suspension of whey protein nanogels. c) Optionally, concentrate the suspension of whey protein nanogel to obtain a concentrated suspension of whey protein nanogel. d) Optionally, dry the dehydrator feed containing the whey protein nanogel derived from step b) or c).

[0008] Another aspect of the invention relates to a method for producing a whey protein nanogel composition, the method comprising: a) To provide a whey protein solution having the following: - A natural BLG content of at least 3% w / w, pH in the range of -5.8 to 7.5, preferably 5.8 to 6.5. -The weight ratio between the total amount of calcium and natural BLG is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * pH -0.0234, but greater than 0, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 25 mM, -If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 20 mM, b) Heat the whey protein solution to a temperature of at least 68°C for a period of time sufficient to form a suspension of whey protein nanogels. c) Optionally, concentrate the suspension of whey protein nanogel to obtain a concentrated suspension of whey protein nanogel. d) Optionally, dry the dehydrator feed containing the whey protein nanogel derived from step b) or c).

[0009] In addition to the above advantages, the inventors observed that the nanogel of the present invention provides remarkably low viscosity when present in a liquid at high protein concentrations, such as 20% w / w or even 30% w / w, and at the same time is stable against heat treatment, including sterilization heat treatment at such protein concentrations.

[0010] Prior art particles of denatured whey protein offer significantly higher viscosity at increased protein concentrations, and may not even be able to reach a 20% w / w protein concentration in liquid solution.

[0011] Therefore, another aspect of the invention relates to a whey protein nanogel composition comprising at least 30% of the total protein in amount of whey protein nanogel, and at least 30% w / w of the total protein in amount of total solids.

[0012] In some preferred embodiments of the present invention, the whey protein nanogel composition is a whey protein nanogel composition in powder form comprising the following: - A whey protein nanogel in an amount of at least 90% w / w relative to total protein, -Soluble whey protein aggregates in an amount of at most 5% w / w relative to total protein, -Total BLG in an amount of at least 90% w / w relative to total protein, and - A total amount of protein of at least 30% of the total solid weight.

[0013] The low viscosity and exceptional thermal stability of these nanogels make them highly suitable for high-protein beverages, enabling the production of heat-sterilized, high-protein beverage products with low viscosity that are therefore easy to drink.

[0014] Therefore, another aspect of the invention relates to a packaged heat-treated beverage having a pH in the range of 3-8 and containing at least 1% w / w of whey protein nanogel. A further aspect relates to a process for producing a packaged, heat-treated beverage.

[0015] Therefore, another aspect of the invention relates to a process for producing an acidic, concentrated food product, comprising the following steps: - A step of preparing a liquid food base having a pH of at least 5.7, wherein the liquid food base comprises a whey protein nanogel composition sufficient to provide a 4-20% w / w amount of protein, and the whey protein nanogel composition preferably comprises the following steps as specified herein: -Soluble whey protein aggregates in an amount of 15-70% w / w relative to total protein, - Whey protein nanogel in an amount of at least 30-85% relative to total protein, - A step of heating the liquid food base at at least 70°C for a period of time sufficient to at least pasteurize the liquid food base. -Optionally, a step of homogenizing a heat-treated liquid food base, - A step to acidify the heat-treated, liquid food base to a pH of at most 5.4. -Optional step of homogenizing the acidified food base Acidic, concentrated foods are mixtures of an acidified food base or an acidified liquid food base and further ingredient components such as sweeteners and / or flavorings.

[0016] Further aspects relate to acidic, concentrated foods that can be obtained by this process.

[0017] Furthermore, one aspect of the invention relates to the use of whey protein nanogel compositions and / or multiple whey protein nanogels as defined herein for one or more of the following: -As a food ingredient, - As a food ingredient for producing a sterile beverage containing at least 10% protein, and more preferably at least 21% protein, pH less than -5.5 and 20°C and 300s -1 As a food ingredient for producing acidic, concentrated foods with a viscosity exceeding 200 cP as measured by the shear rate, and -For example, as a whitening agent in coffee cream.

[0018] A further aspect of the invention relates to the use of whey protein nanogels and / or whey protein nanogel compositions as a protein source for reducing the astringency and / or acidity of a heat-treated protein beverage having a pH of 3.0-5.0, most preferably 3.5-4.6. - Preferably, the whey protein nanogel provides at least 50% w / w of the total protein of the heat-treated beverage, more preferably at least 70% w / w of the total protein of the heat-treated beverage, even more preferably at least 80% w / w, and most preferably at least 90% w / w; and Preferably, the heat-treated beverage contains a total protein content of 2-35% w / w, more preferably 4-30% w / w, even more preferably 6-25% w / w, and more preferably 8-20% w / w. [Brief explanation of the drawing]

[0019] [Figure 1] This shows the distribution of whey protein nanogels and soluble aggregates relative to total protein after heat treatment of a whey protein solution containing 4-16% natural BLG protein and pH 5.9 at 90°C for 14 minutes. [Figure 2] Transmission electron microscope images of whey protein nanogel suspensions prepared as follows are shown: A: 4% w / w natural BLG; B: 8% w / w natural BLG; C: 12% w / w natural BLG; and D: 16% w / w natural BLG. The scale bar is 500 nm for all images. [Figure 3] This shows the viscosity progression during UF enrichment of a 14% w / w whey protein nanogel suspension (black circle) and a natural BLG solution (× mark) up to approximately 30% w / w total protein. [Figure 4] This shows the progression of the storage modulus (gel strength) of whey protein nanogel preparations containing soluble whey protein aggregates ranging from 1.9% (Sample D) to 59.2% (Sample A) relative to total protein. All samples were diluted to 4% total protein before determining the storage modulus. [Modes for carrying out the invention]

[0020] BLG is the most important protein in bovine whey and milk serum, and is present in several genetic variants, with the main ones in milk being classified as A and B. BLG is a lipocalin protein that can bind to many hydrophobic molecules, suggesting a role in their transport. BLG has also been shown to be able to bind to iron via siderofoam, potentially playing a role in the fight against pathogens. Congeners of BLG are deficient in human breast milk.

[0021] Bovine BLG is a relatively small protein consisting of approximately 162 amino acid residues and having a molecular weight of approximately 18.3–18.4 kDa. Under physiological conditions, it is primarily a dimer, but dissociates into monomers below approximately pH 3, and its native state is conserved as determined by nuclear magnetic resonance spectroscopy. Conversely, BLG also occurs in tetrameric, octameric, and other multimeric aggregate forms under various natural conditions.

[0022] In relation to the present invention, the term "natural BLG" refers to unmodified BLG molecules found, for example, in raw milk or whey, or in low-heat BLG isolates prepared, for example, by BLG crystallization, chromatography, or filtration. Therefore, crystalline natural BLG is still natural BLG. The amount of natural BLG is quantified according to Analysis 6.

[0023] In relation to this invention, the term "total BLG" refers to the sum of natural, modified, and aggregated BLG. The amount of total BLG is quantified according to Analysis 17.

[0024] In relation to the present invention, the term "crystal" refers to a solid material in which its constituent elements (e.g., atoms, molecules, or ions) are arranged in a highly ordered microstructure, forming a crystal lattice that extends in all directions.

[0025] In connection with the present invention, the term "BLG crystal" primarily refers to protein crystals containing native BLGs that are not aggregated, preferably arranged in a highly ordered microstructure, and form a crystalline lattice extending in all directions. BLG crystals can be monolithic or polycrystalline, and can be, for example, complete crystals, crystal fragments, or combinations thereof. Crystal fragments are formed, for example, when complete crystals are subjected to mechanical shearing during processing. Crystal fragments also have the highly ordered microstructure of the crystal but may lack the flat surfaces and / or smooth edges or corners of the complete crystal. In either case, BLG crystals or crystal fragments can be visually identified as clearly defined, compact, coherent structures using optical microscopy. BLG crystals or crystal fragments are often at least partially transparent. Protein crystals are also known to be birefringent, and this optical property can be used to identify unknown particles having a crystalline structure.

[0026] In connection with the present invention, the term "edible composition" refers to a composition that is safe for human consumption and use as a food ingredient and does not contain problematic amounts of toxic components, such as toluene or other undesirable organic solvents. The whey protein nanogel composition and food of the present invention are preferably edible foods.

[0027] In connection with the present invention, the terms "ALA" or "α-lactalbumin" refer to α-lactalbumin of mammalian origin, for example, in its natural and / or glycosylated forms, and include naturally occurring genetic variants. The terms further include aggregated ALA and precipitated BLG. When referring to the amount of ALA, the total amount of ALA, including, for example, aggregated ALA, is indicated. The total amount of ALA is determined according to Example 1.31. The term "aggregated ALA" refers to ALA that is typically not at least partially folded and is further aggregated, typically by hydrophobic interactions and / or covalent bonds, with other denatured ALA molecules and / or other denatured whey proteins.

[0028] In connection with the present invention, the terms “caseinomacropeptide” or “CMP” refer to a hydrophilic peptide of mammalian species, e.g., in its natural and / or glycosylated form, derived from the hydrolysis of “κ-CN” or “κ-casein” by aspartate proteinase, e.g., chymosin, e.g., κ-CN or κ-casein), residues 106–169, and include naturally occurring genetic variants.

[0029] In relation to the present invention, the term "BLG isolate" means a composition containing BLG in an amount of at least 85% w / w relative to total protein. The BLG isolate preferably has a total protein content of at least 30% w / w, preferably at least 80% w / w, relative to the total solid.

[0030] The term "whey" refers to the liquid phase remaining after the casein in milk has been precipitated and removed. Casein precipitation can be achieved, for example, by acidifying the milk and / or by using rennet enzymes. There are several types of whey, for example, "sweet whey," which is a whey product produced by the precipitation of casein based on rennet, and "acid whey" or "sour whey," which is a whey product produced by the precipitation of casein based on acid. Precipitation of casein based on acid can be achieved, for example, by adding food acids or by bacterial culture.

[0031] The term "whey" refers to the liquid that remains after casein and milk fat globules have been removed from milk, for example, by microfiltration or large-pore ultrafiltration. Whey is also considered a type of whey and is sometimes called "ideal whey."

[0032] The terms "whey protein" or "serum protein" refer to proteins present in whey.

[0033] In connection with the present invention, the term "whey protein" refers to proteins found in whey or milk serum. Whey protein may be a subset of protein species found in whey or milk serum, and may even be a single whey protein species, or it may be the complete set of protein species found in whey and / or milk serum.

[0034] In connection with the present invention, the terms “liquid” and “solution” encompass both liquid compositions that do not contain particulate matter and liquid compositions that include combinations of liquid and solid and / or semi-solid particles, such as protein crystals or other protein particles. However, “liquid” and “solution” are preferably pumpable.

[0035] In connection with the present invention, the terms "whey protein concentrate" (WPC) and "serum protein concentrate" (SPC) refer to dry or aqueous compositions containing a total amount of protein of 20-89% w / w relative to the total solids.

[0036] WPC or SPC preferably includes the following: 20-89% w / w of protein relative to the total solid, 15-70% w / w BLG relative to total protein, 8-50% w / w of ALA relative to total protein, and CMP at 0-40% w / w relative to the protein.

[0037] Alternatively, and also preferable, the WPC or SPC may include the following: 20-89% w / w of protein relative to the total solid, 15-90% w / w BLG relative to total protein, 4-50% w / w of ALA relative to total protein, and CMP at 0-40% w / w relative to the protein.

[0038] Preferably, the WPC or SPC includes the following: 20-89% w / w of protein relative to the total solid, 15-80% w / w BLG relative to total protein, 4-50% w / w of ALA relative to total protein, and CMP at 0-40% w / w relative to the protein.

[0039] More preferably, the WPC or SPC includes the following: 70-89% w / w of protein relative to the total solid, 30-90% w / w BLG relative to total protein, 4-35% w / w of ALA relative to total protein, and CMP at 0-25% w / w relative to the protein.

[0040] SPC typically contains no CMP or only trace amounts of CMP.

[0041] The terms "whey protein isolate" (WPI) and "serum protein isolate" (SPI) refer to dry or aqueous compositions containing a total amount of protein of 90–100% w / w relative to the total solids.

[0042] WPI or SPI preferably includes the following: 90-100% w / w of protein relative to the total solid, 15-70% w / w BLG relative to total protein, 8-50% w / w of ALA relative to total protein, and CMP at 0-40% w / w relative to total protein.

[0043] Alternatively, and also preferable, WPI or SPI may include the following: 90-100% w / w of protein relative to the total solid, 30-95% w / w BLG relative to total protein, 4-35% w / w of ALA relative to total protein, and CMP at 0-25% w / w relative to total protein.

[0044] More preferably, WPI or SPI may include the following: 90-100% w / w of protein relative to the total solid, 30-90% w / w BLG relative to total protein, 4-35% w / w of ALA relative to total protein, and CMP at 0-25% w / w relative to total protein.

[0045] SPI typically contains no CMP or only trace amounts of CMP.

[0046] In relation to the present invention, the term "whey protein nanogel" refers to nano-sized (typically about 150-1000 nm) particles of denatured whey protein, which are typically spherical or nearly spherical in shape. Whey protein nanogels are also called whey protein micelles, as described, for example, in WO2007 / 110421A2, although their micelle properties are questionable. The amount of whey protein nanogel is quantified according to Analysis 3. When suspended, the protein nanogel has an opaque, milky appearance and is therefore very well suited for opaque beverages.

[0047] In connection with the present invention, the term "soluble whey protein aggregates" refers to small aggregates of denatured whey protein, which can form a strong gel (much stronger than that of natural whey protein) during acidification to pH 4.6, and which typically have a linear, worm-like, branched, or chain-like shape and are typically submicron in size. Soluble whey protein aggregates are well known to those skilled in the art, for example, described in WO2007 / 110421A2, where they are called linear aggregates. The amount of soluble whey protein aggregates is quantified according to Analysis 3. Soluble whey protein aggregates typically form a clear solution when dissolved in water, and are therefore very well suited for clear beverages.

[0048] The terms "consisting essentially of" and "consisting essentially of" mean that the claim or feature in question encompasses those that do not substantially affect the basic and novel characteristics (if any) of the invention claimed, and specific materials or steps.

[0049] In the context of the present invention, the phrase "Y and / or X" means "Y" or "X" or "Y and X". Along the same logical direction, the phrase "n1, n2,..., n i-1 , and / or n i " means "n1" or "n2" or... or "n i-1 " or "n i " or any combination of the following components: n1, n2,... n i-1 , and n i .

[0050] In the context of the present invention, the terms "dried" or "dry" mean that the composition or product in question contains at most 10% w / w of water, preferably at most 6% w / w and more preferably less than that.

[0051] In the context of the present invention, the weight percentage (% w / w) of a component of a certain composition, product, or material means the weight percentage of that component with respect to the weight of the specific composition, product, or material, unless specifically referred to another standard (e.g., total solids or total protein).

[0052] In the context of the present invention, the term "weight ratio" between component X and component Y means the value obtained by calculating m X / m Y , where m X is the amount (weight) of component X and m Y is the amount (weight) of component Y.

[0053] In relation to the present invention, the term "at least pasteurization" refers to a heat treatment that has a microbial killing effect of 10 seconds or more at 70°C. The criterion for determining the bacterial killing effect is Escherichia coli O157:H7.

[0054] In relation to the present invention, the term "sterile" means that the sterile composition or product in question does not contain viable microorganisms and therefore does not experience microbial growth during storage at room temperature. A sterilized composition is sterile.

[0055] When liquids such as beverages are sterilized and packaged sterilely in sterile containers, they typically have a shelf life of at least six months at room temperature. Sterilization kills spores and microorganisms that could cause the liquid to spoil.

[0056] Therefore, one aspect of the invention relates to a method for producing a whey protein nanogel composition, the method comprising the following: a) To provide a whey protein solution having the following: - A natural BLG content of at least 3% w / w, pH in the range of -5.8 to 7.5, preferably 5.8 to 6.5. - The weight ratio between the total amount of calcium and natural BLG is at most 0.010, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 25 mM, -If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 20 mM, b) Heat the whey protein solution to a temperature of at least 68°C for a period of time sufficient to form a suspension of whey protein nanogels. c) Optionally, concentrate the suspension of whey protein nanogel to obtain a concentrated suspension of whey protein nanogel. d) Optionally, dry the dehydrator feed containing the whey protein nanogel derived from step b) or c).

[0057] Another aspect of the invention relates to a method for producing a whey protein nanogel composition, the method comprising: a) To provide a whey protein solution having the following: - A natural BLG content of at least 3% w / w, pH in the range of -5.8 to 7.5, preferably 5.8 to 6.5. -The weight ratio between the total amount of calcium and natural BLG is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * pH -0.0234 but greater than 0, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 25 mM, -If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 20 mM, b) Heat the whey protein solution to a temperature of at least 68°C for a period of time sufficient to form a suspension of whey protein nanogels. c) Optionally, concentrate the suspension of whey protein nanogel to obtain a concentrated suspension of whey protein nanogel. d) Optionally, dry the dehydrator feed containing the whey protein nanogel derived from step b) or c).

[0058] In some preferred embodiments of the present invention, the method provides a whey protein nanogel composition in powder form and comprises steps a), b), c), and d).

[0059] In another preferred embodiment of the present invention, the method provides a whey protein nanogel composition in powder form, comprising steps a), b), and d), but not step c).

[0060] In a more preferred embodiment of the present invention, the method provides a whey protein nanogel composition in liquid form, comprising steps a), b), and c), but not step d).

[0061] In a more preferred embodiment of the present invention, the method provides a whey protein nanogel composition in liquid form, comprising steps a) and b), but not steps c) and d).

[0062] As described above, step a) provides a whey protein solution containing natural BLG and optionally other whey proteins. The whey protein solution is an aqueous solution, preferably containing at least 50% w / w of water. The whey protein solution is preferably edible and suitable as a food. In addition to dissolved protein, the whey protein solution may contain suspended particles.

[0063] The whey protein solution contains at least 3% w / w of natural BLG.

[0064] In some preferred embodiments of the present invention, the whey protein solution contains natural BLG in an amount of at least 4% w / w, more preferably at least 6% w / w, even more preferably at least 8% w / w, and most preferably at least 10% w / w.

[0065] In another preferred embodiment of the present invention, the whey protein solution contains natural BLG in an amount of at least 11% w / w, more preferably at least 16% w / w, even more preferably at least 18% w / w, and most preferably at least 20% w / w.

[0066] In a more preferred embodiment of the present invention, the whey protein solution contains natural BLG in an amount of at least 21% w / w, more preferably at least 23% w / w, even more preferably at least 25% w / w, and most preferably at least 27% w / w.

[0067] Preferably, the whey protein solution contains natural BLG in an amount of 3-30% w / w, more preferably 4-28% w / w, even more preferably 6-26% w / w, and most preferably 8-24% w / w.

[0068] In some preferred embodiments of the present invention, the whey protein solution contains natural BLG in an amount of 11-30% w / w, more preferably 12-28% w / w, even more preferably 14-26% w / w, and most preferably 16-24% w / w.

[0069] In another preferred embodiment of the present invention, the whey protein solution contains natural BLG in an amount of 10-24% w / w, more preferably 12-22% w / w, even more preferably 14-20% w / w, and most preferably 16-18% w / w.

[0070] In a more preferred embodiment of the present invention, the whey protein solution contains natural BLG in an amount of 21-32% w / w, more preferably 22-31% w / w, even more preferably 23-30% w / w, and most preferably 24-29% w / w.

[0071] In some preferred embodiments of the present invention, the whey protein solution contains a total protein amount of at least 4% w / w, more preferably at least 6% w / w, even more preferably at least 8% w / w, and most preferably at least 10% w / w.

[0072] Preferably, the whey protein solution contains a total protein amount of 1-30% w / w, more preferably 4-28% w / w, even more preferably 6-26% w / w, and most preferably 8-24% w / w.

[0073] In some preferred embodiments of the present invention, the whey protein solution contains 11-30% w / w of total protein, more preferably 12-28% w / w, even more preferably 14-26% w / w, and most preferably 16-24% w / w.

[0074] In another preferred embodiment of the present invention, the whey protein solution contains a total protein amount of 10-24% w / w, more preferably 12-22% w / w, even more preferably 14-20% w / w, and most preferably 16-18% w / w.

[0075] In a more preferred embodiment of the present invention, the whey protein solution contains a total protein amount of 21-32% w / w, more preferably 22-31% w / w, even more preferably 23-30% w / w, and most preferably 24-29% w / w.

[0076] In some preferred embodiments of the present invention, the whey protein solution contains a total protein amount of at least 30% w / w of total solids, more preferably at least 60% w / w of total solids, even more preferably at least 70% w / w of total solids, and most preferably at least 80% w / w of total solids.

[0077] In another preferred embodiment of the present invention, the whey protein solution contains a total protein amount of at least 85% w / w, more preferably at least 90% w / w, more preferably at least 92% w / w, and most preferably at least 95% w / w, relative to the total solids.

[0078] In some preferred embodiments of the present invention, the whey protein solution contains natural BLG in an amount of at least 50% w / w, more preferably at least 60% w / w, more preferably at least 70% w / w, and most preferably at least 80% w / w, relative to the total protein.

[0079] In another preferred embodiment of the present invention, the whey protein solution contains natural BLG in an amount of at least 85% w / w of total protein, more preferably at least 90% w / w of total protein, even more preferably at least 92% w / w of total protein, and most preferably at least 95% w / w of total protein. The whey protein solution is often preferably contained in an amount of natural BLG in an amount of at least 97% w / w of total protein.

[0080] In a more preferred embodiment of the present invention, the whey protein solution contains natural BLG in an amount ranging from 50–80% w / w of total protein, more preferably from 52–75% w / w of total protein, even more preferably from 54–70% w / w of total protein, and most preferably from 55–65% w / w of total protein. This is useful, for example, when highly desalted WPI is used as the protein source for the whey protein solution.

[0081] The whey protein solution may contain other proteins besides natural BLG, and typically contains other whey proteins. In some preferred embodiments of the present invention, the whey protein solution contains only proteins derived from mammalian whey.

[0082] In some preferred embodiments of the present invention, the whey protein solution has a degree of protein denaturation of at most 20% w / w of total protein, more preferably at most 10% w / w of total protein, even more preferably at most 5% w / w of total protein, and most preferably at most 2% w / w of total protein.

[0083] Even lower denaturation may be preferable, and in some preferred embodiments of the present invention, the whey protein solution has a degree of protein denaturation of at most 1% w / w of total protein, more preferably at most 0.5% w / w of total protein, even more preferably at most 0.2% w / w of total protein, and most preferably at most 0.1% w / w of total protein.

[0084] The degree of protein denaturation is measured according to Analysis 3.

[0085] In some preferred embodiments of the present invention, the whey protein solution has a total solid content of 3-50% w / w, more preferably 4-40% w / w, even more preferably 6-35% w / w, and most preferably 8-30% w / w.

[0086] In another preferred embodiment of the present invention, the whey protein solution has a total solid content of 10-50% w / w, more preferably 12-40% w / w, even more preferably 14-35% w / w, and most preferably 16-30% w / w.

[0087] In some preferred embodiments of the present invention, the whey protein solution has a water content of 50-97% w / w, more preferably 60-96% w / w, even more preferably 65-94% w / w, and most preferably 70-92% w / w.

[0088] The non-solid portion of the whey protein solution is preferably water.

[0089] The whey protein solution has a pH in the range of 5.8-7.5.

[0090] In some preferred embodiments of the present invention, the whey protein solution has a pH in the range of 5.8-6.5, more preferably 5.9-6.3, and most preferably 5.9-6.2.

[0091] In another preferred embodiment of the present invention, the whey protein solution has a pH in the range of 5.9-6.5, more preferably 6.0-6.4, and most preferably 6.1-6.3.

[0092] In a more preferred embodiment of the present invention, the whey protein solution has a pH in the range of 6.5-7.5, more preferably 6.6-7.2, and even more preferably 6.7-7.0.

[0093] pH adjustment is preferably performed using Na + and K + This is carried out using alkalizing agents that do not increase the content of monovalent metal ions. Ca(OH)2 or amine-based alkalizing agents are currently preferred. Alternatively, the use of an alkalizing agent may include a combination of one or more bases containing monovalent metal ions and one or more bases containing divalent metal ions. Such combinations are useful, for example, when the use of Ca(OH)2 alone for pH adjustment provides too high a weight ratio between calcium and natural BLG, and the resulting concentration of monovalent metal ions does not exceed the threshold required for efficient nanogel formation.

[0094] In some particularly preferred embodiments of the invention, the whey protein solution has a weight ratio between the total amount of calcium and natural BLG, which is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * The pH is -0.0234, but it is greater than 0.

[0095] The term "greater than zero" means that the weight ratio between the total amount of calcium and natural BLG is always greater than absolute zero, because whey protein solution always contains trace amounts of calcium, even if difficult to detect. However, the weight ratio can be very close to zero.

[0096] The total weight of other divalent metals in the whey protein solution is lower than the total weight of calcium, more preferably at most 50% of the total weight of calcium, and most preferably at most 20% of the total weight of calcium.

[0097] In some preferred embodiments of the present invention, the whey protein solution has the following weight ratio between the total amount of calcium and natural BLG: -At most 0.0041 * pH-0.0220, and -At least 0.0037 * The pH is -0.0222, but it is greater than 0.

[0098] In another preferred embodiment of the present invention, the whey protein solution has the following weight ratio between the total amount of calcium and natural BLG: -At most, 0.0040 * pH-0.0221, and -At least 0.0039 * The pH is -0.0221, but it is greater than 0.

[0099] In some preferred embodiments of the present invention, the whey protein solution has a weight ratio between the total amount of calcium and natural BLG of at most 0.0070, more preferably at most 0.0065, even more preferably at most 0.0060, and most preferably at most 0.0050.

[0100] In another preferred embodiment of the present invention, the whey protein solution has a weight ratio between the total amount of calcium and natural BLG of at most 0.0045, more preferably at most 0.0040, even more preferably at most 0.0035, and most preferably at most 0.0030.

[0101] Even lower weight ratios are often preferred, and in some preferred embodiments of the present invention, the whey protein solution has a weight ratio between the total amount of calcium and natural BLG of at most 0.0025, more preferably at most 0.0020, even more preferably at most 0.0015, and most preferably at most 0.0005.

[0102] In some preferred embodiments of the present invention, the whey protein solution has a total calcium content in the range of 0.0005-0.0065, more preferably 0.0010-0.0050, even more preferably 0.0015-0.0040, and most preferably in the range of 0.0015-0.0030, for example, preferably a weight ratio of 0.0017-0.0027 between the total calcium content and natural BLG.

[0103] The whey protein solution further has the following total concentrations of monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 25 mM, - If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 20 mM.

[0104] In some preferred embodiments of the present invention, the natural BLG content of the whey protein solution is less than 10% w / w, and the whey protein solution has a total concentration of monovalent metal cations of at most 24 mM, more preferably at most 22 mM, even more preferably at most 21 mM, and most preferably at most 20 mM.

[0105] In some preferred embodiments of the present invention, regardless of the content of natural BLG, the whey protein solution has a total concentration of monovalent metal cations of at most 19 mM, more preferably at most 17 mM, even more preferably at most 15 mM, and most preferably at most 10 mM. Even lower content of monovalent metal cations may be preferred, and in some preferred embodiments of the present invention, the whey protein solution has a total concentration of monovalent metal cations of at most 8 mM, more preferably at most 6 mM, even more preferably at most 4 mM, and most preferably at most 2 mM.

[0106] This method makes it possible to produce whey protein nanogel compositions with very high yields of whey protein nanogels and low content of often undesirable soluble whey protein aggregates and fine particles. Therefore, this method provides an improved and more cost-effective method for producing whey protein nanogel compositions with high purity whey protein nanogels, enabling the production of novel whey protein nanogel compositions not available in the prior art.

[0107] Whey protein solution may contain other major nutrients besides protein, such as carbohydrates and / or lipids.

[0108] However, it is often preferable that the whey protein solution contains carbohydrates in an amount of at most 15% w / w of the total solids, more preferably at most 5% w / w of the total solids, even more preferably at most 1% w / w of the total solids, and most preferably at most 0.1% w / w of the total solids.

[0109] The whey protein solution more often preferably contains lipids in an amount of at most 8% w / w of total solids, more preferably at most 2% w / w of total solids, even more preferably at most 0.5% w / w of total solids, and most preferably at most 0.1% w / w of total solids.

[0110] Whey protein solutions may contain other major nutrients and material components besides protein. The embodiments and priorities relating to major nutrients and additional material components described below in relation to packaged, heat-treated beverages also apply to whey protein solutions, and we refer to those embodiments instead of repeating them here.

[0111] In some particularly preferred embodiments of the invention, the whey protein solution has the same chemical composition as that of a packaged, heat-treated beverage, except that the protein is in its natural form.

[0112] In another particularly preferred embodiment of the invention, the whey protein solution has the same chemical composition as that of a packaged, heat-treated beverage.

[0113] The protein source for the whey protein solution may be natural BLG and any source that also optionally provides minerals. The whey protein source can be, for example, whey protein isolate, whey protein isolate, whey protein concentrate, or a combination thereof. Whey protein isolate and / or whey protein isolate are particularly preferred. The whey protein source preferably has a very low mineral content.

[0114] Currently preferred whey protein sources are BLG isolates that can be obtained by crystallization and recovery of BLG crystals outlined in WO2018 / 115520A1, i.e., by crystallization of BLG in mode of salting from an aqueous solution containing whey protein and having a pH of 5-6. The protein source may be, for example, a wet crystalline slurry obtained by the process according to WO2018 / 115520A1, or a spray-dried crystalline slurry obtained according to WO2018 / 115520A1. Alternatively, also preferred, the protein source may be BLG isolates that can be obtained by the process outlined in PCT / EP2019 / 066998, preferably PCT / EP2019 / 066998. WO2018 / 115520A1 and PCT / EP2019 / 066998 are incorporated herein by reference for all purposes.

[0115] Alternatively, and this is also preferable, the protein source may be a BLG isolate obtained by de Jongh et al (Mild Isolation Procedure Discloses New Protein Structural Properties of beta-Lactoglobulin, J Dairy Sci., vol. 84(3), 2001, pp. 562-571), which can then be subjected to further desalting by dialysis.

[0116] Alternatively, and this is also preferable, the protein source may be commercially available high-quality WPI, which is subjected to desalting by dialysis before use.

[0117] The whey protein used in the whey protein solution is whey protein derived from mammalian milk, for example, from cow, goat, mare, sheep, camel, and / or buffalo milk. Bovine whey protein is particularly preferred.

[0118] The proteins in the various compositions described herein are preferably edible proteins and may include other edible proteins in addition to BLG. The proteins of the present invention are derived from mammalian milk, and it is particularly preferable that the proteins are provided by isolating and / or modifying one or more protein species derived from mammalian milk, for example. The proteins of the present invention are most preferably whey proteins, or protein materials derived from whey proteins, preferably by heat denaturation. However, it is assumed, and often preferred, that foods containing the whey protein nanogel or whey protein nanogel composition of the present invention may contain non-milk proteins in addition to milk-derived protein species.

[0119] Ideally, a whey protein solution is provided by dissolving a whey protein source in desalinated water and optionally adjusting the pH. Further modification of the mineral composition may be necessary to achieve the useful whey protein solutions described herein.

[0120] Step b) includes heating the whey protein solution to a temperature of at least 68°C for a period of time sufficient to form a suspension of whey protein nanogels. Step b) may further include cooling the suspension to end the heat treatment, for example for direct spray drying or for food production, unless the suspension is to be used warm.

[0121] If step b) includes cooling, the suspension is typically cooled to a temperature of at most 50°C, more preferably at most 40°C, even more preferably at most 20°C, and more preferably at most 10°C.

[0122] In some preferred embodiments of the present invention, the heating in step b) heats the whey protein solution to a temperature of at least 70°C, more preferably at least 75°C, even more preferably at least 80°C, and most preferably at least 85°C. Higher temperatures have been proven useful, and in some preferred embodiments of the present invention, the heating in step b) heats the whey protein solution to a temperature of at least 90°C, more preferably at least 95°C, even more preferably at least 100°C, and most preferably at least 120°C.

[0123] In some preferred embodiments of the present invention, the heating in step b) heats the whey protein solution to a temperature in the range of 68-160°C, more preferably 75-150°C, even more preferably 80-120°C, and most preferably 85-100°C.

[0124] In step b), it is particularly preferable to heat the whey protein solution to a temperature in the range of 80-95°C, more preferably 82-92°C, even more preferably 84-90°C, and most preferably 85-89°C.

[0125] The duration of the heat treatment in step b) must be sufficient to form a substantial amount of nanogel. The duration is preferably at least 500 milliseconds, and often much longer. The duration is preferably chosen to denature a substantial amount of innate BLG in the whey protein solution.

[0126] In some preferred embodiments of the present invention, the heating in step b) is carried out for a period of time sufficient to denature at least 50% w / w of the natural BLG, more preferably at least 80% w / w of the natural BLG, even more preferably at least 90% of the natural BLG, and most preferably at least 95% w / w of the natural BLG. A higher level of BLG denature may be preferable, and in some preferred embodiments of the present invention, the heating in step b) is carried out for a period of time sufficient to denature at least 96% w / w of the natural BLG, more preferably at least 97% w / w of the natural BLG, even more preferably at least 98% of the natural BLG, and most preferably at least 99% w / w of the natural BLG.

[0127] The inventors found that a high level of BLG denaturation provides better thermal stability to the resulting whey protein nanogel composition.

[0128] The duration of the heat treatment depends on the temperature, but is typically 1 minute to 1 hour, preferably 4-50 minutes, more preferably 6-45 minutes, even more preferably 8-40 minutes, and most preferably 10-30 minutes.

[0129] Surprisingly, this method makes it possible to produce whey protein nanogel compositions at high protein concentrations, with only limited mechanical shear, or even without mechanical shear, regardless of the relatively high protein concentrations used in whey protein solutions. In some preferred embodiments of the present invention, the heat treatment in step b) does not involve mechanical shear, for example, a scraped surface heat exchanger or high-pressure homogenization. However, mechanical shear is not excluded from the present invention, and in other preferred embodiments of the present invention, the heat treatment in step b) includes mechanical shear.

[0130] The compositional characteristics described in relation to the whey protein solution in step a) are similarly applicable to the suspension of whey protein nanogel obtained in step b), except that a considerable amount of native protein has been denatured and thus converted into, for example, whey protein nanogel.

[0131] Step c) is optional, but is preferred in some embodiments.

[0132] Therefore, in some preferred embodiments of the present invention, the method includes step c) concentrating a suspension of whey protein nanogels to obtain a concentrated suspension of whey protein nanogels.

[0133] However, in another preferred embodiment of the present invention, the method does not include step c), and therefore the suspension is not concentrated.

[0134] In this document, the term "concentrating a suspension of whey protein nanogels" includes, but does not include, a drying step such as spray drying, at least removing water to increase the concentration of the whey protein nanogels.

[0135] The suspension of whey protein nanogels is preferably concentrated by one or more of the following methods: microfiltration, ultrafiltration, nanofiltration, reverse osmosis, and / or evaporation. Ultrafiltration, nanofiltration, or reverse osmosis are particularly preferred because they preserve the protein content of the suspension.

[0136] In some embodiments of the present invention, the concentration in step c) increases the content of the whey protein nanogel in the suspension by at least 25%, more preferably at least 50%, even more preferably at least 75%, and most preferably at least 100%. Higher levels of concentration may be required, and in some preferred embodiments of the present invention, the concentration in step c) increases the content of the whey protein nanogel in the suspension by at least 200%, more preferably at least 300%, even more preferably at least 500%, and most preferably at least 700%.

[0137] In some embodiments of the present invention, the concentration in step c) increases the content of the whey protein nanogel in the suspension by 25-900%, more preferably 100-850%, even more preferably 200-825%, and most preferably 300-800%.

[0138] In some preferred embodiments of the present invention, the concentration in step c) provides a concentrated suspension of whey protein nanogel containing a total amount of protein of at least 21% w / w, more preferably at least 25%, even more preferably at least 28% w / w, and most preferably at least 30% w / w.

[0139] Therefore, in some preferred embodiments of the present invention, the concentrated suspension of whey protein nanogel contains a total amount of protein of at least 21% w / w, more preferably at least 25%, even more preferably at least 28% w / w, and most preferably at least 30% w / w.

[0140] In another preferred embodiment of the present invention, the concentration in step c) provides a concentrated suspension of whey protein nanogel containing a total amount of protein of 21-35% w / w, more preferably 25-33%, even more preferably 28-32% w / w, and most preferably 29-31% w / w.

[0141] Therefore, in another preferred embodiment of the present invention, the concentrated suspension of whey protein nanogel contains a total amount of protein of 21-35% w / w, more preferably 25-33%, even more preferably 28-32% w / w, and most preferably 29-31% w / w.

[0142] In some preferred embodiments of the present invention, the concentration in step c) provides a concentrated suspension of whey protein nanogel containing an amount of at least 21% w / w, more preferably at least 25%, even more preferably at least 28% w / w, and most preferably at least 30% w / w of whey protein nanogel.

[0143] Therefore, in some preferred embodiments of the present invention, the concentrated suspension of whey protein nanogel contains at least 21% w / w, more preferably at least 25%, even more preferably at least 28% w / w, and most preferably at least 30% w / w of whey protein nanogel.

[0144] In another preferred embodiment of the present invention, the concentration in step c) provides a concentrated suspension of whey protein nanogel containing an amount of whey protein nanogel in the range of 21-35% w / w, more preferably 25-33%, even more preferably 28-32% w / w, and most preferably 29-31% w / w.

[0145] Therefore, in another preferred embodiment of the present invention, the concentrated suspension of whey protein nanogel contains an amount of whey protein nanogel of 21-35% w / w, more preferably 25-33%, even more preferably 28-32% w / w, and most preferably 29-31% w / w.

[0146] The inventors have found that it is preferable to control the content of soluble whey protein aggregates in the suspension and concentrated suspension and to maintain them at a minimum level.

[0147] Therefore, in some preferred embodiments of the present invention, the concentrated suspension of whey protein nanogel contains at most 8% w / w, more preferably at most 6%, even more preferably at most 3% w / w, and most preferably at most 1% w / w of soluble whey protein aggregates. Even lower content of soluble whey protein aggregates is achievable, and in some preferred embodiments of the present invention, the concentrated suspension of whey protein nanogel contains at most 1% w / w, more preferably at most 0.5%, even more preferably at most 0.3% w / w, and most preferably at most 0.1% w / w of soluble whey protein aggregates.

[0148] In some preferred embodiments of the present invention, the concentrated suspension of whey protein nanogel contains whey protein nanogel in an amount of at least 60% w / w, more preferably at least 70% w / w, even more preferably at least 80% w / w, and most preferably at least 90% w / w of total protein.

[0149] Even higher content of whey protein nanogel is achievable and often preferred. Therefore, in some preferred embodiments of the present invention, the concentrated suspension of whey protein nanogel contains at least 92% w / w of whey protein nanogel relative to total protein, more preferably at least 94% w / w, even more preferably at least 96% w / w, and most preferably at least 98% w / w of total protein.

[0150] The compositional characteristics described in relation to the whey protein solution in step a) are similarly applicable to the concentrated suspension of whey protein nanogel obtained in step c), except that a considerable amount of native protein has been denatured and thus converted into, for example, whey protein nanogel. Furthermore, the total protein content was increased for concentration.

[0151] If the pH of the whey protein nanogel composition differs from the pH used during the formation of the whey protein nanogel, the method preferably comprises one or more steps of adjusting the pH of one or more whey protein nanogel-containing streams, e.g., suspensions of whey protein nanogels, concentrated suspensions of whey protein nanogels, and / or dryer feeds obtained by or in accordance with step b). One or more pH adjustments are sufficient to provide a whey protein nanogel composition having a desired pH, preferably one of the preferred ranges mentioned in relation to the whey protein nanogel composition. One or more pH adjustments preferably use one or more suitable acids or bases, preferably selected from the acids or bases mentioned herein.

[0152] Step d) is optional, but is preferred in some embodiments.

[0153] In some preferred embodiments of the present invention, the method does not include step d), and the drying step is not performed.

[0154] However, in other preferred embodiments of the present invention, the method includes step d), which comprises drying a dryer feed comprising a whey protein nanogel derived from step b) or c). Step d) is particularly preferred because it provides a whey protein nanogel composition in powder form that is easy to transport and has better storage stability than an aqueous suspension.

[0155] In relation to the present invention, the term “dryer feed” refers to a liquid feed supplied to a dryer for conversion of the feed into a powder. The dryer feed comprises the whey protein nanogel produced in step b).

[0156] In some preferred embodiments of the present invention, the dryer feed comprises the solid of the whey protein nanogel suspension of step b) and / or the solid of the concentrated whey protein nanogel suspension of step c).

[0157] In another preferred embodiment of the present invention, the dryer feed solid comprises the solid of the whey protein nanogel suspension of step b) and / or the solid of the concentrated whey protein nanogel suspension of step c).

[0158] In some preferred embodiments of the present invention, the dryer feed is a suspension of the whey protein nanogel from step b) and / or a concentrated suspension of the whey protein nanogel from step c).

[0159] Preferably, the dryer feed contains a total amount of protein of at least 21% w / w, more preferably at least 25%, even more preferably at least 28% w / w, and most preferably at least 30% w / w.

[0160] In some preferred embodiments of the present invention, the dryer feed contains a total amount of protein of 21-35% w / w, more preferably 25-33%, even more preferably 28-32% w / w, and most preferably 29-31% w / w.

[0161] In another preferred embodiment of the present invention, the dryer feed contains a total amount of protein of 15-32% w / w, more preferably 17-31%, even more preferably 18-30% w / w, and most preferably 19-29% w / w.

[0162] Preferably, the dryer feed contains at least 21% w / w, more preferably at least 25%, even more preferably at least 28% w / w, and most preferably at least 30% w / w of whey protein nanogel.

[0163] In some preferred embodiments of the present invention, the dryer feed comprises 21-35% w / w, more preferably 25-33%, even more preferably 28-32% w / w, and most preferably 29-31% w / w of whey protein nanogel.

[0164] In another preferred embodiment of the present invention, the dryer feed comprises whey protein nanogel in an amount of 10-35% w / w, more preferably 12-30%, even more preferably 14-25% w / w, and most preferably 15-20% w / w.

[0165] The inventors observed that drying a dehydrator feed containing 10-25% w / w of whey protein nanogel provides a dried whey protein nanogel composition with improved dispersibility when reconstituted in water. Therefore, in some preferred embodiments of the invention, the dehydrator feed contains 10-25% w / w, more preferably 12-25%, even more preferably 14-20% w / w, and most preferably 15-20% w / w of whey protein nanogel.

[0166] The dryer feed preferably contains at most 8% w / w, more preferably at most 6%, even more preferably at most 3% w / w, and most preferably at most 1% w / w of soluble whey protein aggregates.

[0167] In some preferred embodiments of the present invention, the dryer feed contains whey protein nanogel in an amount of at least 60% w / w, more preferably at least 70% w / w, even more preferably at least 80% w / w, and most preferably at least 90% w / w of total protein.

[0168] Higher content of whey protein nanogels is achievable and often preferred. Therefore, in some preferred embodiments of the present invention, the dehydrator feed contains whey protein nanogels in an amount of at least 92% w / w, more preferably at least 94% w / w, even more preferably at least 96% w / w, and most preferably at least 98% w / w of total protein.

[0169] In some preferred embodiments of the present invention, the dryer feed includes the following: - A total BLG content of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. Total solid content in the range of -21-40% w / w, most preferably 24-35% w / w. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein.

[0170] In a more preferred embodiment of the present invention, the dryer feed includes the following: - A total BLG content of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. Total solid content in the range of -8-25% w / w, most preferably 12-22% w / w. - Whey protein nanogel in an amount of 30-85% w / w, most preferably 35-70% w / w, relative to total protein, and -Soluble whey protein aggregates in an amount of 15-70% w / w, most preferably 30-65% w / w, relative to total protein.

[0171] In a more preferred embodiment of the present invention, the dryer feed includes the following: - A total BLG content of at least 50% w / w, most preferably at least 60% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. Total solid content in the range of -8-25% w / w, most preferably 12-22% w / w. - Whey protein nanogel in an amount of 30-85% w / w, most preferably 35-70% w / w, relative to total protein, and -Soluble whey protein aggregates in an amount of 15-70% w / w, most preferably 30-65% w / w, relative to total protein.

[0172] The dryer feed is particularly preferably to contain carbohydrates in an amount of at most 15% w / w of the total solids, more preferably at most 5% w / w of the total solids, even more preferably at most 1% w / w of the total solids, and most preferably at most 0.1% w / w of the total solids.

[0173] In some preferred embodiments of the invention, the dehydrator feed contains carbohydrates in an amount ranging from 1–15% w / w, more preferably 5–15% w / w, and most preferably 8–15% w / w, relative to the total solids. The inventors have observed that such embodiments are useful for whey protein nanogel compositions in powder form, because they are considered to be easily reconstituted and hydrated in powder form. The carbohydrates preferably include, or are composed of, digestible carbohydrates such as sucrose, lactose, glucose, galactose and / or maltodextrin, for example.

[0174] Carbohydrates may be present in the whey protein solution before the heat treatment in step b). However, in some preferred embodiments of the invention, at least some of the carbohydrates in the dryer feed are added after the heat treatment in step b).

[0175] It is even more preferable that the dryer feed contains lipids in an amount of at most 8% w / w of the total solids, more preferably at most 2% w / w of the total solids, even more preferably at most 0.5% w / w of the total solids, and most preferably at most 0.1% w / w of the total solids.

[0176] In some preferred embodiments of the present invention, the method is a method for producing a whey protein nanogel composition in powder form, and the method includes the following: a) To provide a whey protein solution having the following: -8-30% w / w, most preferably 12-24% w / w of natural BLG content, - A content of natural BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. pH in the range of -5.8 to 7.5, most preferably 5.8 to 6.5. - The weight ratio between total calcium and natural BLG is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * pH -0.0234, but greater than 0, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 20 mM, most preferably at most 15 mM, or -If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 15 mM, most preferably at most 10 mM. b) Heating the whey protein solution to a temperature of 80-100°C, most preferably at least 85-95°C, for a period of time sufficient to form a suspension of whey protein nanogels, the period of time being sufficient to denature at least 90%, most preferably at least 95%, of the natural BLG. c) Optionally, concentrate the suspension of whey protein nanogel to obtain a concentrated suspension of whey protein nanogel. d) Drying the dryer feed by spray drying, wherein the dryer feed comprises a whey protein nanogel derived from step b) or c), preferably the dryer feed is a suspension from step b) or a concentrated suspension from step c).

[0177] In some preferred embodiments of the present invention, the method is a method for producing a whey protein nanogel composition in powder form, and the method includes the following: a) To provide a whey protein solution having the following: -8-30% w / w, most preferably 12-24% w / w of natural BLG content, - A content of natural BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. pH in the range of -5.8 to 7.5, most preferably 5.8 to 6.5. -The weight ratio between the total amount of calcium and natural BLG is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * pH -0.0234, but greater than 0, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 20 mM, most preferably at most 15 mM, or -If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 15 mM, most preferably at most 10 mM. b) Heating the whey protein solution to a temperature of 80-100°C, most preferably at least 85-95°C, for a period of time sufficient to form a suspension of whey protein nanogels, the period of time being sufficient to denature at least 90%, most preferably at least 95%, of the natural BLG. c) If the concentration of whey protein nanogel in the suspension from step b) is less than the required whey protein nanogel concentration from step d), concentrate the whey protein nanogel suspension to obtain a concentrated whey protein nanogel suspension having the required whey protein nanogel concentration. d) Drying the dryer feed by spray drying, wherein the dryer feed comprises whey protein nanogel derived from step b) or c), preferably the dryer feed is a suspension of step b) or a concentrated suspension of step c), and the dryer feed comprises the following: - A total BLG content of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. Total solid content in the range of -21-40% w / w, most preferably 24-35% w / w. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein.

[0178] In some preferred embodiments of the present invention, the method is a method for producing a whey protein nanogel composition in powder form, and the method includes the following: a) To provide a whey protein solution having the following: -16-30% w / w, most preferably 18-24% w / w of natural BLG content, - A content of natural BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. pH in the range of -5.8 to 7.5, most preferably 5.8 to 6.5. -The weight ratio between the total amount of calcium and natural BLG is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * pH -0.0234, but greater than 0, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 20 mM, most preferably at most 15 mM, or -If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 15 mM, most preferably at most 10 mM. b) Heating the whey protein solution to a temperature of 80-100°C, most preferably at least 85-95°C, for a period of time sufficient to form a suspension of whey protein nanogels, the period of time being sufficient to denature at least 90%, most preferably at least 95%, of the natural BLG. d) Drying the dryer feed by spray drying, wherein the dryer feed contains whey protein nanogel derived from step b) or c), and the dryer feed is a suspension of step b).

[0179] In some preferred embodiments of the present invention, the method is a method for producing a whey protein nanogel composition in powder form, and the method includes the following: a) To provide a whey protein solution having the following: -3-10% w / w, most preferably 4-8% w / w of natural BLG content, - A content of natural BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. pH in the range of -5.8 to 7.5, most preferably 5.8 to 6.5. -The weight ratio between the total amount of calcium and natural BLG is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * pH -0.0234, but greater than 0, and -Total concentration of the following monovalent metal cations: -At most 15 mM, most preferably at most 10 mM, b) Heating the whey protein solution to a temperature of 80-100°C, most preferably at least 85-95°C, for a period of time sufficient to form a suspension of whey protein nanogels, the period of time being sufficient to denature at least 90%, most preferably at least 95%, of the natural BLG. c) Concentrate the whey protein nanogel suspension to obtain a concentrated whey protein nanogel suspension having the whey protein nanogel concentration required in step d). d) Drying the dryer feed by spray drying, wherein the dryer feed comprises whey protein nanogel derived from step b) or c), the dryer feed is a concentrated suspension of step c), and the dryer feed comprises the following: - A total BLG content of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. Total solid content in the range of -21-40% w / w, most preferably 24-35% w / w. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein.

[0180] The whey protein nanogel composition is particularly preferably to contain carbohydrates in an amount of at most 15% w / w of the total solids, more preferably at most 5% w / w of the total solids, even more preferably at most 1% w / w of the total solids, and most preferably at most 0.1% w / w of the total solids.

[0181] In some preferred embodiments of the invention, the whey protein nanogel composition contains carbohydrates in an amount ranging from 1–15% w / w, more preferably 5–15% w / w, and most preferably 8–15% w / w, relative to the total solids. The inventors have observed that such embodiments are useful for whey protein nanogel compositions in powder form, since the reconstitution and hydration of the powder are considered to be easy. The carbohydrates preferably include, or are composed of, digestible carbohydrates such as sucrose, lactose, glucose, galactose, and / or maltodextrin.

[0182] The whey protein nanogel composition is more preferably to contain lipids in an amount of at most 8% w / w of total solids, more preferably at most 2% w / w of total solids, even more preferably at most 0.5% w / w of total solids, and most preferably at most 0.1% w / w of total solids.

[0183] In some preferred embodiments of the present invention, the method is a method for producing a whey protein nanogel composition in powder form, and the method includes the following: a) To provide a whey protein solution having the following: -8-20% w / w, most preferably 12-18% w / w of natural BLG content, - A content of natural BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. pH in the range of -5.8 to 7.5, most preferably 5.9 to 6.5. -The weight ratio between the total amount of calcium and natural BLG is as follows: -At most 0.0041 * pH-0.0209, and -At least 0.0037 * pH -0.0234, but greater than 0, and -Total concentration of the following monovalent metal cations: -If the natural BLG content of the whey protein solution is less than 10% w / w, then 18-25 mM, most preferably 20-25 mM, or -If the natural BLG content of the whey protein solution is at least 10% w / w, then 15-20 mM, most preferably 17-20 mM, b) Heating the whey protein solution to a temperature of 80-100°C, most preferably at least 85-95°C, for a period of time sufficient to form a suspension of whey protein nanogels, the period of time being sufficient to denature at least 90%, most preferably at least 95%, of the natural BLG. c) Optionally, concentrate the suspension of whey protein nanogel to obtain a concentrated suspension of whey protein nanogel. d) Drying the dryer feed by spray drying, wherein the dryer feed comprises whey protein nanogel derived from step b) or c), preferably the dryer feed is a suspension of step b) or a concentrated suspension of step c), and preferably the dryer feed comprises the following: - A total BLG content of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. -Total protein content of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. Total solid content in the range of -8-25% w / w, most preferably 12-22% w / w. - Whey protein nanogel in an amount of 30-85% w / w, most preferably 35-70% w / w, relative to total protein, and -Soluble whey protein aggregates in an amount of 15-70% w / w, most preferably 30-65% w / w, relative to total protein.

[0184] Furthermore, one aspect of the invention relates to a whey protein nanogel composition comprising at least 30% of the total protein in amount of whey protein nanogel and at least 30% w / w of the total protein in amount of total solids. The whey protein nanogel composition can preferably be obtained by the method described herein.

[0185] In some preferred embodiments of the present invention, the whey protein nanogel composition comprises whey protein nanogel in an amount of at least 60% w / w, more preferably at least 70% w / w, even more preferably at least 80% w / w, and most preferably at least 90% w / w of total protein.

[0186] A higher content of whey protein nanogel is often preferred, and in another preferred embodiment of the present invention, the whey protein nanogel composition contains at least 92% w / w, more preferably at least 94% w / w, even more preferably at least 96% w / w, and most preferably at least 98% w / w of total protein in amount of whey protein nanogel.

[0187] Furthermore, it is preferable that the whey protein nanogel composition contains whey protein nanogel in an amount of approximately 100% w / w relative to the total protein.

[0188] In some preferred embodiments of the present invention, the whey protein nanogel composition contains soluble whey protein aggregates in an amount of at most 30% w / w, more preferably at most 20% w / w, even more preferably at most 10% w / w, and most preferably at most 5% w / w of total protein, relative to the total protein.

[0189] A lower content of soluble whey protein aggregates is often preferred, and the whey protein nanogel composition preferably contains at most 3% w / w, more preferably at most 2% w / w, even more preferably at most 1% w / w, and most preferably at most 0.5% w / w of soluble whey protein aggregates based on the total protein.

[0190] In another preferred embodiment of the present invention, the whey protein nanogel composition contains at most 30% w / w, more preferably at most 20% w / w, even more preferably at most 10% w / w, and most preferably at most 5% w / w of soluble whey protein aggregates based on the total weight of the composition.

[0191] A lower content of soluble whey protein aggregates is often preferred, and the whey protein nanogel composition preferably contains at most 3% w / w, more preferably at most 2% w / w, even more preferably at most 1% w / w, and most preferably at most 0.5% w / w of soluble whey protein aggregates based on the total weight of the composition.

[0192] Whey protein nanogel compositions having a low content of soluble whey protein aggregates are particularly useful in high-protein acidic beverages.

[0193] The inventors have observed signs that such whey protein nanogel compositions having an increased content of whey protein nanogels are subjected to slower gastrointestinal digestion and form less gel in the acidic environment of the stomach than soluble whey protein aggregates. Therefore, whey protein nanogels are considered to contribute less to the development of structure and satiety than soluble whey protein aggregates. This makes these whey protein nanogels useful for high-energy beverages for clinical nutrition at any pH that do not promote satiety.

[0194] The inventors have observed that a whey protein nanogel composition having a significant content of soluble whey protein aggregates is stable to heat treatment and forms a further gel upon acidification. Thus, such a whey protein nanogel composition is highly suitable for acidic, thick foods produced by pasteurizing a liquid food base and then acidifying the heat-treated food base. This is useful for replacing the use of carbohydrate-based hydrocolloids such as starch, gums or pectin, for example.

[0195] In some preferred embodiments of the present invention, the whey protein nanogel composition comprises: - a total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, based on the total protein, - an amount of whey protein nanogel of 30 - 85% w / w, most preferably 35 - 70% w / w, based on the total protein, and - an amount of soluble whey protein aggregates of 15 - 70% w / w, most preferably 30 - 65% w / w, based on the total protein.

[0196] In other preferred embodiments of the present invention, the whey protein nanogel composition comprises: - a total amount of BLG of at least 50% w / w, most preferably at least 60% w / w, based on the total protein, - an amount of whey protein nanogel of 30 - 85% w / w, most preferably 35 - 70% w / w, based on the total protein, and - an amount of soluble whey protein aggregates of 15 - 70% w / w, most preferably 30 - 65% w / w, based on the total protein.

[0197] The inventors have observed indications that such whey protein nanogel compositions having an increased content of soluble whey protein aggregates are likely to be more readily digested in the gastrointestinal tract, forming a gel in the acidic environment of the stomach, which is thought to contribute to structural development and satiety. Therefore, these whey protein nanogel compositions may be useful in beverages that can promote improved satiety and / or rapid protein digestion.

[0198] A whey protein nanogel composition containing soluble whey protein aggregates in an amount of 15-70% w / w, most preferably 30-65% w / w, relative to total protein, is prepared at a pH of less than 5.5 and at 20°C and 300s. -1 It can be used as a food ingredient to produce thick foods with a viscosity exceeding 200 cP, as measured by the shear rate.

[0199] The whey protein nanogel composition of the present invention is typically preferred to contain a small amount of larger whey protein particles, which may cause sedimentation and, furthermore, a sandy texture in beverages. Therefore, in some preferred embodiments of the present invention, the whey protein nanogel composition contains whey protein microparticles in an amount of at most 10% w / w, more preferably at most 5% w / w, even more preferably at most 3% w / w, and most preferably at most 1% w / w of total protein relative to the total protein. The content of whey protein microparticles is determined according to Analysis 3.

[0200] The whey protein nanogel composition of this embodiment typically contained less than 4% w / w of whey protein microparticles, if present.

[0201] In some preferred embodiments of the present invention, the whey protein nanogel composition contains at least 30% w / w of total protein relative to the total solids, more preferably at least 60% w / w of total solids, even more preferably at least 70% w / w of total solids, and most preferably at least 80% w / w of total protein relative to the total solids.

[0202] In another preferred embodiment of the present invention, the whey protein nanogel composition contains a total protein amount of at least 85% w / w, more preferably at least 90% w / w, more preferably at least 92% w / w, and most preferably at least 95% w / w, relative to the total solids.

[0203] In some preferred embodiments of the present invention, the whey protein nanogel composition contains a total protein amount of at least 30% w / w, more preferably at least 60% w / w, even more preferably at least 70% w / w, and most preferably at least 80% w / w.

[0204] In another preferred embodiment of the present invention, the whey protein nanogel composition contains a total protein amount of at least 85% w / w, more preferably at least 90% w / w, even more preferably at least 92% w / w, and most preferably at least 95% w / w.

[0205] In some preferred embodiments of the present invention, the whey protein nanogel composition contains a total amount of BLG in an amount of at least 50% w / w, more preferably at least 60% w / w, even more preferably at least 70% w / w, and most preferably at least 80% w / w, relative to the total protein.

[0206] In another preferred embodiment of the present invention, the whey protein nanogel composition contains total BLG in an amount of at least 85% w / w, more preferably at least 90% w / w, even more preferably at least 92% w / w, and most preferably at least 95% w / w, relative to the total protein. The whey protein nanogel composition is often preferably to contain total BLG in an amount of at least 97% w / w, relative to the total protein.

[0207] In a more preferred embodiment of the present invention, the whey protein nanogel composition contains a total amount of BLG in the range of 50-80% w / w relative to the total protein, more preferably in the range of 52-75% w / w relative to the total protein, even more preferably in the range of 54-70% w / w relative to the total protein, and most preferably in the range of 55-65% w / w relative to the total protein.

[0208] In connection with the present invention, the terms "total amount of BLG" and "total amount of BLG" are used interchangeably and both refer to the total amount of BLG in the composition in question, including both natural and modified BLG.

[0209] In some preferred embodiments of the present invention, the whey protein nanogel composition is liquid and contains a total solid amount of 1-50% w / w, more preferably 10-45% w / w, even more preferably 15-40% w / w, and most preferably 20-35% w / w.

[0210] If the whey protein nanogel composition is a liquid, it is preferable that it contains 50-99% w / w of water, more preferably 55-90% w / w, even more preferably 60-85% w / w, and most preferably 65-80% w / w.

[0211] In relation to the liquid whey protein nanogel composition, it is preferable that soluble whey protein aggregates are present in an amount of at most 8% w / w, more preferably at most 6%, even more preferably at most 3% w / w, and most preferably at most 1% w / w.

[0212] In some preferred embodiments of the present invention, the whey protein nanogel composition is a powder and contains a total solid amount of 90-99% w / w, more preferably 92-99% w / w, even more preferably 94-99% w / w, and most preferably 95-99% w / w.

[0213] When the whey protein nanogel composition is in powder form, it preferably contains water in an amount of 1-10% w / w, more preferably 1-8% w / w, even more preferably 1-6% w / w, and most preferably 1-5% w / w.

[0214] In some preferred embodiments of the present invention, the whey protein nanogel composition is a paste and contains total solids in an amount of 51-89% w / w, more preferably 55-90% w / w, even more preferably 60-85% w / w, and most preferably 65-80% w / w.

[0215] When the whey protein nanogel composition is in powder form, it preferably contains water in an amount of 11-49% w / w, more preferably 13-45% w / w, even more preferably 15-40% w / w, and most preferably 20-35% w / w.

[0216] A wide range of pH is possible, but the whey protein nanogel composition preferably has a pH in the range of 3-8, more preferably 4-7, even more preferably 5-7, and most preferably 6-7.

[0217] When the whey protein nanogel composition contains a significant amount of soluble whey protein aggregates, the pH is preferably in the range of 5.7-8, most preferably in the range of 6.0-7.5.

[0218] The inventors have found that the pH-neutral variant of the whey protein nanogel composition is suitable for pH-neutral food applications, in which case the pH of the final food, such as a beverage, is close to the pH of the whey protein nanogel composition. This reduces the risk of undesirable protein aggregation during protein handling, especially during pH adjustment.

[0219] In some preferred embodiments of the present invention, the whey protein nanogel composition has a pH in the range of 6-8, most preferably 6-7. In other preferred embodiments of the present invention, the whey protein nanogel composition has a pH in the range of 7-8.

[0220] In a more preferred embodiment of the present invention, the whey protein nanogel composition has a pH in the range of 6.5-8.0, more preferably 6.6-7.5, even more preferably 6.8-7.5, and most preferably 6.9-7.5.

[0221] Similar to the situation with the pH-neutral variant of the whey protein nanogel composition, the inventors have found that the acidic variant of the whey protein nanogel composition is particularly suitable for acidic food applications, in which case the pH of the final food, such as a beverage, is close to the pH of the whey protein nanogel composition, thereby reducing the risk of undesirable protein aggregation during protein handling, especially during pH adjustment.

[0222] In some preferred embodiments of the present invention, the whey protein nanogel composition has a pH in the range of 3-5, most preferably 3-4.

[0223] In another preferred embodiment of the present invention, the whey protein nanogel composition has a pH in the range of 4-5.

[0224] In a more preferred embodiment of the present invention, the whey protein nanogel composition has a pH in the range of 3-5.5, more preferably 3.0-5.0, even more preferably 3.0-4.7, and most preferably 3.5-4.5.

[0225] The nanogels of the present invention typically have particle sizes in the nanoscale range. In some preferred embodiments of the present invention, the particles of the hydrated whey protein nanogel composition have a z-mean diameter measured by dynamic light scattering of 150-1000 nm, more preferably 170-900 nm, even more preferably 200-800 nm, and most preferably 250-700 nm.

[0226] In some preferred embodiments of the present invention, the particles of the hydrated whey protein nanogel composition have a z-average diameter of 150-800 nm, more preferably 250-700 nm, even more preferably 300-600 nm, and most preferably 350-500 nm.

[0227] When the nanogel is provided in the form of a powdered whey protein nanogel composition, measuring the particle size and polydispersity index requires reconstitution and hydration of the whey protein nanogel in water before particle size measurement, and preferably, the reconstituted whey protein nanogel is subjected to homogenization to ensure that it is properly hydrated.

[0228] In some preferred embodiments of the present invention, the particles of the whey protein nanogel composition have a polydispersity index of at most 0.3, more preferably at most 0.2, even more preferably at most 0.1, and most preferably at most 0.05.

[0229] If the whey protein nanogel composition is prepared, for example, by directly drying the suspension of whey protein nanogel in step b) or the concentrated suspension in step c), it will contain the same or slightly less minerals based on total solids as the whey protein solution contained.

[0230] Therefore, in some preferred embodiments of the present invention, the whey protein nanogel composition has a weight ratio between the total amount of calcium and natural BLG of at most 0.0070, more preferably at most 0.0065, even more preferably at most 0.0060, and most preferably at most 0.0050.

[0231] In another preferred embodiment of the present invention, the whey protein nanogel composition has a weight ratio of at most 0.0045, more preferably at most 0.0040, even more preferably at most 0.0035, and most preferably at most 0.0030 between the total amount of calcium and the total BLG.

[0232] Even lower weight ratios are often preferred, and in some preferred embodiments of the present invention, the whey protein nanogel composition has a weight ratio of at most 0.0025, more preferably at most 0.0020, even more preferably at most 0.0015, and most preferably at most 0.0010 between the total amount of calcium and the total amount of BLG.

[0233] In another preferred embodiment of the present invention, the whey protein nanogel composition has a weight ratio between the total amount of calcium and the total BLG in the range of 0.0010-0.0030, most preferably in the range of 0.0017-0.0027.

[0234] The whey protein nanogel composition may have a total concentration of monovalent metal cations of at most 20 mM, more preferably at most 15 mM, even more preferably at most 10 mM, and more preferably at most 5 mM, when standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water.

[0235] In some preferred embodiments of the present invention, the whey protein nanogel composition has a total content of monovalent metal ions of at most 0.5% w / w, more preferably at most 0.3% w / w, even more preferably at most 0.1% w / w, and most preferably at most 0.01% w / w, relative to the total solids.

[0236] This method limits the weight ratio between calcium and natural BLG during the heat treatment in step b), but it is possible to enhance the resulting whey protein nanogel suspension with calcium and other minerals. This may be advantageous, for example, if the whey protein nanogel composition is to be used to enhance the mineral content of food.

[0237] Therefore, in some preferred embodiments of the present invention, the whey protein nanogel composition has a weight ratio of at least 0.005, more preferably at least 0.01, even more preferably at least 0.02, and most preferably at least 0.03, between the total amount of calcium and the total BLG.

[0238] In another preferred embodiment of the present invention, the whey protein nanogel composition has a weight ratio of 0.005-0.050, more preferably 0.010-0.045, even more preferably 0.015-0.040, and most preferably 0.020-0.035 between the total amount of calcium and the total BLG.

[0239] In some preferred embodiments of the present invention, the whey protein nanogel composition, when standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, has a total concentration of monovalent metal cations greater than 20 mM, more preferably at least 25 mM, even more preferably at least 50 mM, and more preferably at least 100 mM.

[0240] In another preferred embodiment of the present invention, the whey protein nanogel composition, when standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, has a total concentration of monovalent metal cations of 20-400 mM, more preferably at least 40-350 mM, even more preferably 50-300 mM, and most preferably 60-250 mM.

[0241] The whey protein nanogel composition may contain other major nutrients besides protein, such as carbohydrates and / or lipids.

[0242] However, whey protein nanogel compositions often preferably contain carbohydrates in an amount of at most 15% w / w of total solids, more preferably at most 5% w / w of total solids, even more preferably at most 1% w / w of total solids, and most preferably at most 0.1% w / w of total solids.

[0243] In some preferred embodiments of the invention, the whey protein nanogel composition contains carbohydrates in an amount ranging from 1–15% w / w, more preferably 5–15% w / w, and most preferably 8–15% w / w, relative to the total solids. The inventors have observed that such embodiments are useful for whey protein nanogel compositions in powder form, since the reconstitution and hydration of the powder are considered to be easy. The carbohydrates preferably include, or are composed of, digestible carbohydrates such as sucrose, lactose, glucose, galactose and / or maltodextrin.

[0244] The whey protein nanogel composition more often contains lipids in an amount of at most 8% w / w of total solids, more preferably at most 2% w / w of total solids, even more preferably at most 0.5% w / w of total solids, and most preferably at most 0.1% w / w of total solids.

[0245] Whey protein nanogel compositions may contain other major nutrients and material components besides protein. The embodiments and priorities relating to major nutrients and additional material components described below in relation to packaged heat-treated beverages also apply to whey protein nanogel compositions, and we refer to those embodiments instead of repeating them here.

[0246] In some particularly preferred embodiments of the invention, the whey protein nanogel composition has the same chemical composition as a packaged heat-treated beverage, except that the protein is in its natural form.

[0247] In another particularly preferred embodiment of the invention, the whey protein nanogel composition has the same chemical composition as the packaged heat-treated beverage.

[0248] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0249] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 70% w / w, most preferably at least 80% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, more preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0250] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 80% w / w, most preferably at least 85% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 20% w / w, most preferably at most 15% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0251] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 70% w / w, most preferably at least 80% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0252] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - Whey protein nanogel in an amount of 30-85% w / w, most preferably 35-70% w / w, relative to total protein, and - Soluble whey protein aggregates in an amount of 15-70% w / w, most preferably 30-65% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0253] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - Whey protein nanogel in an amount of 30-59% w / w, most preferably 35-50% w / w, relative to total protein, and - Soluble whey protein aggregates in an amount of 21-50% w / w, most preferably 30-45% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0254] The powder of the present invention is preferably dried by spray drying.

[0255] In some preferred embodiments of the present invention, the whey protein nanogel composition is in liquid form, and the whey protein nanogel composition comprises the following: -Total protein in an amount of 21-35% w / w, most preferably 24-32% w / w, relative to the total weight of the whey protein nanogel composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. -Total BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0256] In some preferred embodiments of the present invention, when a whey protein nanogel composition in liquid form is standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, it is subjected to 20°C and 300 s. -1 The shear rate is at most 200 cP, more preferably 20°C and 300 s -1 The shear rate is at most 100 cP, and more preferably 20°C and 300 s -1 The shear rate is at most 50 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 20 cP at a shear rate.

[0257] Other methods can be used to prepare this whey protein nanogel composition, but it is preferable that the whey protein nanogel composition be obtained by the method described herein.

[0258] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0259] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 70% w / w, most preferably at least 80% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, more preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0260] In another preferred embodiment of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, more preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0261] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 80% w / w, most preferably at least 85% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 20% w / w, most preferably at most 15% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0262] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 70% w / w, most preferably at least 80% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0263] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0264] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - Whey protein nanogel in an amount of 30-85% w / w, most preferably 35-70% w / w, relative to total protein, and - Soluble whey protein aggregates in an amount of 15-70% w / w, most preferably 30-65% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0265] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - Whey protein nanogel in an amount of 30-59% w / w, most preferably 35-50% w / w, relative to total protein, and - Soluble whey protein aggregates in an amount of 21-50% w / w, most preferably 30-45% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0266] The powder of the present invention is preferably dried by spray drying.

[0267] In some preferred embodiments of the present invention, the whey protein nanogel composition is in liquid form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: -Total protein in an amount of 21-35% w / w, most preferably 24-32% w / w, relative to the total weight of the whey protein nanogel composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. -Total BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0268] In some preferred embodiments of the present invention, the whey protein nanogel composition is in liquid form and has a pH in the range of 6-8, most preferably 7-8, and the whey protein nanogel composition comprises the following: -Total protein in an amount of 21-35% w / w, most preferably 24-32% w / w, relative to the total weight of the whey protein nanogel composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. -Total BLG in an amount of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 55% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0269] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0270] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 70% w / w, most preferably at least 80% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, more preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0271] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, more preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 150 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 100 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0272] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 80% w / w, most preferably at least 85% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 20% w / w, most preferably at most 15% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0273] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 70% w / w, most preferably at least 80% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0274] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range. ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 The shear rate is at most 300 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0275] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - Whey protein nanogel in an amount of 30-85% w / w, most preferably 35-70% w / w, relative to total protein, and - Soluble whey protein aggregates in an amount of 15-70% w / w, most preferably 30-65% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0276] In some preferred embodiments of the present invention, the whey protein nanogel composition is in powder form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: - An amount of total solids of at least 92% w / w, most preferably at least 94% w / w, relative to the total weight of the composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - Whey protein nanogel in an amount of 30-59% w / w, most preferably 35-50% w / w, relative to total protein, and - Soluble whey protein aggregates in an amount of 21-50% w / w, most preferably 30-45% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0277] The powder of the present invention is preferably dried by spray drying.

[0278] In some preferred embodiments of the present invention, the whey protein nanogel composition is in liquid form and has a pH in the range of 3-5, most preferably 3-4, and the whey protein nanogel composition comprises the following: -Total protein in an amount of 21-35% w / w, most preferably 24-32% w / w, relative to the total weight of the whey protein nanogel composition. -Total protein in an amount of at least 80% w / w, most preferably at least 90% w / w, relative to the total solids. -Total BLG in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein. In addition, one or more of the following: i) The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the 150-900 nm range, and ii) When standardized to 20% w / w total protein by vacuum evaporation or addition of milli-Q water, 20°C and 300 s -1 It has a viscosity of at most 200 cP at a shear rate, and iii) The particles of the hydrated whey protein nanogel composition have a polydispersity index of at most 0.2.

[0279] The whey protein nanogel composition is preferably prepared by thermal denaturation of whey protein at one of the preferred subranges of pH in the range of 5.8-7.5 or in relation to the whey protein solution of step a).

[0280] Furthermore, one aspect of the invention relates to whey protein nanogels that can be obtained by the methods described herein. Individual whey protein nanogels can be separated, for example, by microfiltration, fractionation centrifugation, and density gradient centrifugation.

[0281] Multiple hydrated whey protein nanogels preferably have a z-average diameter of 150-1000 nm, more preferably 170-900 nm, even more preferably 200-800 nm, and most preferably 250-700 nm.

[0282] In some preferred embodiments of the present invention, the hydrated form of the whey protein nanogels has a z-average diameter of 150-800 nm, more preferably 250-700 nm, even more preferably 300-600 nm, and most preferably 350-500 nm.

[0283] In some preferred embodiments of the present invention, the whey protein nanogel is present in desalinated water at a concentration of 20.0% w / w, and is subjected to 20°C and 300s. -1 The shear rate is at most 200 cP, more preferably 20°C and 300 s -1 The shear rate is at most 100 cP, and more preferably 20°C and 300 s -1 The shear rate is at most 50 cP, most preferably 20°C and 300 s -1 It provides a viscosity of at most 40 cP at a shear rate.

[0284] In some preferred embodiments of the present invention, the hydrated form of the whey protein nanogels has a polydispersity index of at most 0.3, more preferably at most 0.2, and most preferably at most 0.1.

[0285] Furthermore, one aspect of the present invention relates to a food product comprising a whey protein nanogel composition or a plurality of whey protein nanogels as defined herein.

[0286] The food is preferably converted into a product that includes a whey protein nanogel composition or a whey protein nanogel plus at least one additional material component, and / or is no longer a whey protein nanogel composition.

[0287] The food is preferably a beverage, an acidic concentrated food, or a solid food.

[0288] The inventors have found that the whey protein nanogel and whey protein nanogel composition are particularly useful in beverages and, preferably, packaged, heat-treated beverages having a high protein content.

[0289] Therefore, a particular aspect of the invention relates to a packaged, heat-treated beverage containing at least whey protein nanogel.

[0290] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a pH in the range of 3–8 and contains at least 1% w / w of whey protein nanogel.

[0291] The whey protein nanogel for beverages is preferably provided by a whey protein nanogel composition as defined herein, or is particularly preferably a whey protein nanogel as defined herein. It is even more particularly preferred that the whey protein nanogel for beverages can be obtained by a method described herein.

[0292] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains a total protein amount in the range of 1-32% w / w, more preferably 5-31% w / w, even more preferably 10-30% w / w, and most preferably 21-30% w / w.

[0293] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains a total protein amount in the range of 17-32% w / w, more preferably 21-31% w / w, even more preferably 22-30% w / w, and most preferably 24-30% w / w.

[0294] In another preferred embodiment of the present invention, the packaged heat-treated beverage contains a total protein amount in the range of 8-32% w / w, more preferably 9-24% w / w, even more preferably 10-22% w / w, and most preferably 11-20% w / w.

[0295] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains total BLG in an amount of at least 50% w / w of total protein, more preferably at least 60% w / w of total protein, even more preferably at least 70% w / w of total protein, and most preferably at least 80% w / w of total protein.

[0296] In another preferred embodiment of the present invention, the packaged heat-treated beverage contains total BLG in an amount of at least 85% w / w of total protein, more preferably at least 90% w / w of total protein, even more preferably at least 92% w / w of total protein, and most preferably at least 95% w / w of total protein. The whey protein nanogel composition often preferably contains total BLG in an amount of at least 97% w / w of total protein.

[0297] In a more preferred embodiment of the present invention, the packaged heat-treated beverage contains a total amount of BLG in the range of 50-80% w / w relative to total protein, more preferably in the range of 52-75% w / w relative to total protein, even more preferably in the range of 54-70% w / w relative to total protein, and most preferably in the range of 55-65% w / w relative to total protein.

[0298] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains whey protein nanogel in an amount of at least 5% w / w, more preferably at least 8% w / w, even more preferably at least 10% w / w, and most preferably at most at least 11% w / w.

[0299] Preferably, the packaged heat-treated beverage may contain whey protein nanogel in an amount of 5-32% w / w, more preferably 8-24% w / w, even more preferably 10-22% w / w, and most preferably at most 11-20% w / w.

[0300] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains whey protein nanogel in an amount of at least 21% w / w, more preferably at least 22% w / w, even more preferably at least 25% w / w, and most preferably at least 28% w / w.

[0301] Preferably, the packaged heat-treated beverage contains 21-32% w / w, more preferably 22-31% w / w, even more preferably 23-30% w / w, and most preferably 24-30% w / w of whey protein nanogel.

[0302] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains whey protein nanogel in an amount of at least 50% w / w, more preferably at least 70% w / w, even more preferably at least 80% w / w, and most preferably at least 90% w / w of total protein. A higher content of whey protein nanogel is often preferred, and in other preferred embodiments of the present invention, the packaged heat-treated beverage contains whey protein nanogel in an amount of at least 92% w / w, more preferably at least 94% w / w, even more preferably at least 96% w / w, and most preferably at least 98% w / w of total protein.

[0303] The degree of BLG denaturation of the beverage is preferably very high. In some preferred embodiments of the present invention, the packaged heat-treated beverage has a BLG denaturation of at least 70%, more preferably at least 80%, even more preferably at least 85%, and most preferably at least 90% of the total protein. An even higher degree of BLG denaturation is often preferred, and in other preferred embodiments of the present invention, the packaged heat-treated beverage has a BLG denaturation of at least 92%, more preferably at least 94%, even more preferably at least 96%, and most preferably at least 98%.

[0304] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains soluble whey protein aggregates in an amount of at most 30% w / w, more preferably at most 20% w / w, even more preferably at most 10% w / w, and most preferably at most 5% w / w of total protein.

[0305] Even lower content of soluble whey protein aggregates is often preferred, and packaged heat-treated beverages preferably contain soluble whey protein aggregates in an amount of at most 3% w / w, more preferably at most 2% w / w, even more preferably at most 1% w / w, and most preferably at most 0.5% w / w of total protein.

[0306] In another preferred embodiment of the present invention, the packaged heat-treated beverage contains soluble whey protein aggregates in an amount of at most 8% w / w, more preferably at most 5% w / w, even more preferably at most 2% w / w, and most preferably at most 0.5% w / w of the total weight of the beverage.

[0307] The packaged heat-treated beverage of the present invention is typically preferred to contain a small amount of larger whey protein particles that may cause sedimentation and, furthermore, a sandy texture in the beverage. Therefore, in some preferred embodiments of the present invention, the packaged heat-treated beverage contains whey protein microparticles in an amount of at most 10% w / w, more preferably at most 5% w / w, even more preferably at most 3% w / w, and most preferably at most 1% w / w of total protein relative to the total protein. The content of whey protein microparticles is determined according to Analysis 3.

[0308] In some preferred embodiments of the present invention, the packaged heat-treated beverage includes: - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein.

[0309] In another preferred embodiment of the present invention, the packaged heat-treated beverage includes: - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 85% w / w, most preferably at least 89% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0310] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a total solid content of 3-50% w / w, more preferably 4-40% w / w, even more preferably 6-35% w / w, and most preferably 8-30% w / w.

[0311] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a total solid content of 10-50% w / w, more preferably 12-40% w / w, even more preferably 14-35% w / w, and most preferably 16-30% w / w.

[0312] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a water content of 50-97% w / w, more preferably 60-96% w / w, even more preferably 65-94% w / w, and most preferably 70-92% w / w.

[0313] The non-solid, packaged, heat-treated beverage portion is preferably water.

[0314] The pH of a beverage can range from acidic to slightly alkaline.

[0315] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a pH in the range of 5.5–8.0, more preferably 6.0–7.5, even more preferably 6.2–7.3, and most preferably 6.3–7.2.

[0316] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 6.0–7.5, more preferably 6.2–7.5, and most preferably 6.3–7.5.

[0317] In a more preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 6.0–8.0, more preferably 6.6–7.7, even more preferably 6.7–7.6, and most preferably 6.8–7.5.

[0318] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 3.0–5.4, more preferably 3.5–5.0, even more preferably 3.7–4.8, and most preferably 4.0–4.6.

[0319] In a more preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 3.0–5.4, more preferably 3.0–5.0, even more preferably 3.5–5.0, and most preferably 3.5–4.6.

[0320] In a more preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 3.0-5.4, more preferably 3.1-5.0, even more preferably 3.2-4.6, and most preferably 3.5-4.0.

[0321] The inventors found that the viscosity contribution of soluble whey protein aggregates becomes less significant below pH 4.0. Therefore, in some preferred embodiments of the invention, the packaged heat-treated beverage has a pH in the range of 3.0–4.0, more preferably 3.0–3.8, and most preferably 3.0–3.6. Preferably, the packaged heat-treated beverage can have a pH in the range of 3.0–4.0, more preferably 3.0–3.8, and most preferably 3.0–3.6; furthermore, the whey protein nanogel can contribute 50–95% w / w, more preferably 55–85% w / w, and even more preferably 60–75% w / w of the total protein in the packaged heat-treated beverage; and furthermore, the soluble whey protein aggregate can contribute 5–50% w / w, more preferably 15–45% w / w, and most preferably 25–30% w / w of the total protein in the packaged heat-treated beverage.

[0322] The inventors further found that a high content of whey protein nanogel relative to total protein makes it possible to produce a low-viscosity, high-protein beverage with a pH range of 4.0–5.0, most preferably 4.2–4.8. Thus, in some preferred embodiments of the invention, the packaged heat-treated beverage has a pH in the range of 4.0–5.0, most preferably 4.2–4.8. Preferably, the packaged heat-treated beverage can have a pH in the range of 4.0–5.0, most preferably 4.2–4.8, and the whey protein nanogel can contribute at least 80% w / w, most preferably at least 90% w / w, of the total protein in the packaged heat-treated beverage.

[0323] The inventors observed that a heat-treated, acidic protein beverage containing this whey protein nanogel surprisingly had less astringency than comparable beverages containing other types of denatured whey protein. This is demonstrated, for example, in Example 8. This is advantageous, for example, for beverages subjected to protein denaturation heat treatment, such as heat treatment at temperatures above 100°C.

[0324] The advantage of this packaged, heat-treated beverage is that it has a surprisingly low viscosity relative to the amount of protein it contains.

[0325] In some preferred embodiments of the present invention, packaged heat-treated beverages are heated at 20°C and 300s -1 The shear rate is at most 200 cP, more preferably 20°C and 300 s -1 The shear rate is at most 100 cP, more preferably 20°C and 300 s -1 The shear rate is at most 50 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 20 cP at a shear rate.

[0326] Even lower viscosity is possible and often desirable. Therefore, in another preferred embodiment of the present invention, the packaged heat-treated beverage is heated to 20°C and 300s. -1At a shear rate of at most 15 cP, more preferably 20°C and 300 s -1 At a shear rate of at most 10 cP, more preferably 20°C and 300 s -1 The shear rate is at most 8 cP, most preferably 20°C and 300 s -1 It has a viscosity of at most 5 cP at a shear rate.

[0327] Packaged, heat-treated beverages are particularly preferably sterile.

[0328] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a shelf life at ambient temperature of at least 6 months, more preferably at least 1 year, and even more preferably at least 2 years.

[0329] The packaged, heat-treated beverage of the present invention may contain other major nutrients besides protein, such as carbohydrates and / or lipids.

[0330] In some embodiments of the invention, the packaged heat-treated beverage further contains carbohydrates. The total carbohydrate content in the heat-treated beverage of the invention depends on the intended use of the heat-treated beverage.

[0331] The carbohydrates in packaged, heat-treated beverages are preferably provided by one or more sources of carbohydrates.

[0332] Useful carbohydrate sources can be selected from the group consisting of: sucrose, maltose, dextrose, galactose, maltodextrin, corn syrup solids, scromalt, glucose polymers, corn syrup, modified starch, indigestible starch, rice-derived carbohydrates, isomaltulose, white sugar, glucose, fructose, lactose, high-fructose corn syrup, honey, sugar alcohols, fructooligosaccharides, soy fiber, corn fiber, guar gum, konjac powder, polydextrose, fibersol, and combinations thereof. In some embodiments of the invention, the packaged heat-treated beverage contains indigestible sugars such as fructans, and the fructans contain inulin or fructooligosaccharides.

[0333] In some preferred embodiments of the invention, the packaged heat-treated beverage contains carbohydrates in the range of 0-95% of the total energy content of the beverage, more preferably in the range of 10-85%, even more preferably in the range of 20-75%, and most preferably in the range of 30-60%.

[0334] Even lower carbohydrate content is often preferred, and therefore in some preferred embodiments of the invention, it is preferably in the range of 0 to 30% of the total energy content of the beverage, more preferably in the range of 0 to 20% of the total energy content of the beverage, and even more preferably in the range of 0 to 10% of the total energy content of the beverage.

[0335] In some preferred embodiments of the present invention, the beverage is particularly useful as a sports drink and contains, for example, a total amount of carbohydrates of at most 75%, more preferably at most 40E%, even more preferably at most 10E%, and most preferably at most 5E%, of the total energy content (E) of the beverage.

[0336] In some preferred embodiments of the present invention, packaged heat-treated beverages are particularly useful as nutritionally incomplete dietary supplements, for example, containing a total amount of carbohydrates in the range of 70-95%, preferably 80-90E%, of the total energy content (E) of the beverage.

[0337] In some preferred embodiments of the present invention, the packaged heat-treated beverage contains a total amount of carbohydrates ranging from 30-60% of the total energy content of the beverage, most preferably ranging from 35-50%. Such beverages are particularly useful as nutritionally complete beverages.

[0338] In some embodiments of the invention, the packaged heat-treated beverage further comprises at least one additional material component selected from the group consisting of vitamins, flavorings, minerals, sweeteners, antioxidants, dietary acids, lipids, carbohydrates, prebiotics, probiotics, and non-whey proteins, as well as combinations thereof.

[0339] Additional ingredients can be used to adjust the nutritional contribution and taste and flavor characteristics of the beverage.

[0340] In one embodiment of the invention, the beverage contains at least one high-intensity sweetener (HIS). The at least one HIS is preferably selected from the group consisting of aspartame, cyclamic acid, sucralose, acesulfame salt, neotame, saccharin, stevia extract, steviol glycosides such as rebaudioside A, or combinations thereof.

[0341] In some embodiments of the invention, the sweetener is particularly preferably composed of one or more high-intensity sweeteners.

[0342] HIS is found among both natural and artificial sweeteners and typically has a sweetness level at least 10 times that of sucrose.

[0343] When used, the total amount of HIS in the beverage is typically in the range of 0.001–2% w / w. Preferably, the total amount of HIS is in the range of 0.005–1% w / w. Most preferably, the total amount of HIS is in the range of 0.01–0.5% w / w.

[0344] The choice of sweetener may depend on the resulting beverage; for example, high-intensity sweeteners (e.g., aspartame, acesulfame-K, or sucralose) may be used in beverages where an energy contribution from the sweetener is not desired, while natural sweeteners (e.g., steviol glycosides, sorbitol, or sucrose) may be used in beverages with a natural profile.

[0345] The sweetener may more preferably contain, or be composed of, one or more polyol sweeteners. Non-limiting examples of useful polyol sweeteners include maltitol, mannitol, lactitol, sorbitol, inositol, xylitol, treitol, galactitol, or combinations thereof. When used, the total amount of polyol sweetener in the beverage is typically in the range of 1-20% w / w. More preferably, the total amount of polyol sweetener in the beverage is in the range of 2-15% w / w. Even more preferably, the total amount of polyol sweetener may be in the range of 4-10% w / w.

[0346] In some preferred embodiments of the invention, the packaged heat-treated beverage includes: - A total amount of carbohydrates of at most 1% w / w, more preferably at most 0.5% w / w, and most preferably at most 0.1% w / w, and The total amount of HIS in the range of -0.001-2% w / w, more preferably in the range of 0.005-1% w / w, and most preferably in the range of 0.01-0.5% w / w.

[0347] In some embodiments of the invention, the packaged heat-treated beverage further contains lipids. The total lipid content in the heat-treated beverage of the invention depends on the intended use of the heat-treated beverage.

[0348] In some preferred embodiments of the invention, the packaged heat-treated beverage has a lipid content of 0-50% of the total energy content of the beverage, preferably in the range of 0-40%, preferably in the range of 0-30%, preferably in the range of 0-20%, preferably in the range of 0-10%, and preferably in the range of 0-5%.

[0349] In some preferred embodiments of the present invention, the beverage is particularly useful as a sports drink and contains, for example, a total amount of lipids of at most 10E%, preferably at most 1E%.

[0350] In some preferred embodiments of the present invention, packaged heat-treated beverages are particularly useful as nutritionally incomplete dietary supplements, for example, containing a total amount of lipids of at most 10%, preferably at most 1E%, of the total energy content of the beverage.

[0351] In some preferred embodiments of the present invention, a beverage in the form of a sports drink includes, for example, the following: -Total amount of protein in the range of 1-30% w / w relative to the weight of the beverage, more preferably 4-24% w / w relative to the weight of the beverage, even more preferably 8-20% w / w relative to the weight of the beverage, and most preferably 10-20% w / w relative to the weight of the beverage. -The total amount of carbohydrates is at most 75%, more preferably at most 40E%, even more preferably at most 10E%, and most preferably at most 5E%, of the total energy content (E) of the beverage, and - A total amount of lipids of at most 10E%, more preferably at most 6E%, even more preferably at most 3E%, and most preferably at most 1E%.

[0352] In another preferred embodiment of the present invention, for example, a beverage in the form of a low-carbohydrate sports drink includes the following: -Total amount of protein in the range of 1-30% w / w relative to the weight of the beverage, more preferably 4-24% w / w relative to the weight of the beverage, even more preferably 8-20% w / w relative to the weight of the beverage, and most preferably 10-20% w / w relative to the weight of the beverage. -Total amount of carbohydrates of at most 10E%, more preferably at most 6E%, even more preferably at most 3E%, and most preferably at most 1E%, - A total amount of lipids of at most 5E%, more preferably at most 4E%, even more preferably at most 3E%, and most preferably at most 1E%, and The total amount of HIS in the range of -0.001-2% w / w, more preferably in the range of 0.005-1% w / w, and most preferably in the range of 0.01-0.5% w / w.

[0353] In other preferred embodiments of the present invention, for example, a packaged, heat-treated beverage in the form of a nutritionally complete beverage includes: -Total amount of protein in the range of 1-30% w / w relative to the weight of the beverage, more preferably 4-24% w / w relative to the weight of the beverage, even more preferably 8-20% w / w relative to the weight of the beverage, and most preferably 10-20% w / w relative to the weight of the beverage. -Total amount of carbohydrates in the range of 30-60% of the total energy content of the beverage, most preferably in the range of 35-50%. -Total amount of lipids in the range of 20-50% of the total energy amount, more preferably in the range of 25-45%, and most preferably 30-40%.

[0354] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a pH in the range of 3.0–5.4, most preferably 3.5–4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 85% w / w, most preferably at least 89% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0355] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 3.0–5.4, most preferably 3.5–4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 10% w / w, most preferably at most 5% w / w, relative to the total protein.

[0356] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a pH in the range of 3.0–5.4, most preferably 3.5–4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0357] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 3.0–5.4, most preferably 3.5–4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 10% w / w, most preferably at most 5% w / w, relative to the total protein.

[0358] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a pH in the range of 6.2–7.5, most preferably 6.8–7.5, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 85% w / w, most preferably at least 89% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0359] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 6.2–7.5, most preferably 6.8–7.5, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 10% w / w, most preferably at most 5% w / w, relative to the total protein.

[0360] In some preferred embodiments of the present invention, the packaged heat-treated beverage has a pH in the range of 6.2–7.5, most preferably 6.8–7.5, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0361] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 6.2–7.5, most preferably 6.8–7.5, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the beverage, most preferably in the range of 10-22% w / w relative to the weight of the beverage. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 10% w / w, most preferably at most 5% w / w, relative to the total protein.

[0362] In some preferred embodiments of the present invention, a beverage in the form of a sports drink includes, for example, the following: -The total amount of carbohydrates is at most 75%, more preferably at most 40E%, even more preferably at most 10E%, and most preferably at most 5E%, of the total energy content (E) of the beverage, and - A total amount of lipids of at most 10E%, more preferably at most 6E%, even more preferably at most 3E%, and most preferably at most 1E%.

[0363] In other preferred embodiments of the present invention, for example, a packaged, heat-treated beverage in the form of a nutritionally complete beverage includes: -Total amount of carbohydrates in the range of 30-60% of the total energy content of the beverage, most preferably in the range of 35-50%. -Total amount of lipids in the range of 20-50% of the total energy amount, more preferably in the range of 25-45%, and most preferably 30-40%.

[0364] One aspect of the invention relates to a process for producing a packaged, heat-treated beverage having a pH in the range of 3-8, and includes the following steps: 1) Provide a liquid solution having a pH in the range of 3-8 and containing the following: -1 to 32% by weight of total protein (at least 50 w / w% of the protein is β-lactoglobulin (BLG)) -Optionally, sweeteners and / or flavorings 2) Packaging liquid solutions, The liquid solution from step a) and / or the packaged liquid solution from step b) are subjected to a heat treatment, which includes at least pasteurization.

[0365] Therefore, a heat-treated beverage is a heat-treated liquid solution.

[0366] In some particularly preferred embodiments of the invention, the liquid solution is a whey protein solution according to step a) of the above method for producing a whey protein nanogel composition, and the heat treatment in the process for producing a packaged heat-treated beverage is step b) of the above method. The heat treatment is preferably sterilizing, thus enabling the sterile liquid whey protein nanogel composition to be packaged as a heat-treated liquid solution in step 2) of the process for producing a packaged heat-treated beverage.

[0367] In another particularly preferred embodiment of the invention, the liquid solution is as follows: -A suspension of nanogels obtained from step b) of the above method for generating a whey protein nanogel composition, and / or - Concentrated suspension of nanogel obtained from step c), The heat treatment in the process of producing packaged, heat-treated beverages sterilizes the liquid solution or packaged liquid solution.

[0368] In some preferred embodiments, the liquid solution has a pH in the range of 3–8 and contains at least 1% w / w of whey protein nanogel.

[0369] The whey protein nanogels in liquid solution are preferably provided by a whey protein nanogel composition in powder form, and / or, particularly preferably, by a whey protein nanogel as defined herein. It is even more particularly preferred that the whey protein nanogels in liquid solution can be obtained by the method described herein. Providing the liquid solution typically involves reconstituting a whey protein nanogel composition in powder form in water, and, if necessary, homogenizing the reconstituted whey protein nanogel composition until sufficient dispersion is obtained. Preferably, the particle size of the whey protein nanogels in liquid solution is substantially the same as their particle size before drying step d).

[0370] In some preferred embodiments of the present invention, the liquid solution contains a total protein in an amount ranging from 1-32% w / w, more preferably 5-31% w / w, even more preferably 10-30% w / w, and most preferably 21-30% w / w.

[0371] In some preferred embodiments of the present invention, the liquid solution contains a total protein in an amount ranging from 17–32% w / w, more preferably 21–31% w / w, even more preferably 22–30% w / w, and most preferably 24–30% w / w.

[0372] In another preferred embodiment of the present invention, the liquid solution contains a total protein in an amount ranging from 8–32% w / w, more preferably 9–24% w / w, even more preferably 10–22% w / w, and most preferably 11–20% w / w.

[0373] In some preferred embodiments of the present invention, the liquid solution contains total BLG in an amount of at least 50% w / w of total protein, more preferably at least 60% w / w of total protein, even more preferably at least 70% w / w of total protein, and most preferably at least 80% w / w of total protein.

[0374] In another preferred embodiment of the present invention, the liquid solution contains total BLG in an amount of at least 85% w / w of total protein, more preferably at least 90% w / w of total protein, even more preferably at least 92% w / w of total protein, and most preferably at least 95% w / w of total protein. The whey protein nanogel composition is often preferably to contain total BLG in an amount of at least 97% w / w of total protein.

[0375] In a more preferred embodiment of the present invention, the liquid solution contains a total amount of BLG in the range of 50-80% w / w relative to the total protein, more preferably in the range of 52-75% w / w relative to the total protein, even more preferably in the range of 54-70% w / w relative to the total protein, and most preferably in the range of 55-65% w / w relative to the total protein.

[0376] In some preferred embodiments of the present invention, the liquid solution contains whey protein nanogel in an amount of at least 5% w / w, more preferably at least 8% w / w, even more preferably at least 10% w / w, and most preferably at most 11% w / w.

[0377] Preferably, the liquid solution may contain whey protein nanogel in an amount of 5-32% w / w, more preferably 8-24% w / w, even more preferably 10-22% w / w, and most preferably at most 11-20% w / w.

[0378] In some preferred embodiments of the present invention, the liquid solution contains whey protein nanogel in an amount of at least 21% w / w, more preferably at least 22% w / w, even more preferably at least 25% w / w, and most preferably at least 28% w / w.

[0379] Preferably, the liquid solution contains whey protein nanogel in an amount of 21-32% w / w, more preferably 22-31% w / w, even more preferably 23-30% w / w, and most preferably 24-30% w / w.

[0380] In some preferred embodiments of the present invention, the liquid solution contains whey protein nanogel in an amount of at least 50% w / w, more preferably at least 70% w / w, even more preferably at least 80% w / w, and most preferably at least 90% w / w of total protein relative to the total protein. Higher content of whey protein nanogel is often preferred, and in other preferred embodiments of the present invention, the liquid solution contains whey protein nanogel in an amount of at least 92% w / w, more preferably at least 94% w / w, even more preferably at least 96% w / w, and most preferably at least 98% w / w of total protein relative to the total protein.

[0381] In particular, when the proteins in the liquid solution are mainly in the form of whey protein nanogels and optionally soluble whey protein aggregates, the degree of BLG denaturation of the liquid solution is often very high. In some preferred embodiments of the present invention, the liquid solution has a degree of BLG denaturation of at least 70%, more preferably at least 80%, even more preferably at least 85%, and most preferably at least 90% of the total protein. An even higher degree of BLG denaturation is often preferred, and in other preferred embodiments of the present invention, the liquid solution has a degree of BLG denaturation of at least 92%, more preferably at least 94%, even more preferably at least 96%, and most preferably at least 98%.

[0382] In some preferred embodiments of the present invention, the liquid solution contains soluble whey protein aggregates in an amount of at most 30% w / w, more preferably at most 20% w / w, even more preferably at most 10% w / w, and most preferably at most 5% w / w of total protein, relative to the total protein.

[0383] Even lower content of soluble whey protein aggregates is often preferred, and the liquid solution preferably contains soluble whey protein aggregates in an amount of at most 3% w / w, more preferably at most 2% w / w, even more preferably at most 1% w / w, and most preferably at most 0.5% w / w of total protein.

[0384] In another preferred embodiment of the present invention, the liquid solution contains soluble whey protein aggregates in an amount of at most 8% w / w, more preferably at most 5% w / w, even more preferably at most 2% w / w, and most preferably at most 0.5% w / w of the total weight of the liquid solution, relative to the total weight of the liquid solution.

[0385] In some preferred embodiments of the present invention, the liquid solution includes the following: - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 9% w / w, most preferably at most 5% w / w, relative to total protein.

[0386] The liquid solution is typically preferable to contain a small amount of larger whey protein particles, which may cause sedimentation and, furthermore, a sandy texture in the beverage. Therefore, in some preferred embodiments of the present invention, the liquid solution contains whey protein microparticles in an amount of at most 10% w / w, more preferably at most 5% w / w, even more preferably at most 3% w / w, and most preferably at most 1% w / w of total protein.

[0387] The pH of a liquid solution can range from acidic to weakly alkaline.

[0388] For the production of a nearly pH-neutral beverage, a nearly pH-neutral liquid solution is particularly preferred. In some preferred embodiments of the present invention, the liquid solution has a pH in the range of 5.5-8.0, more preferably 6.0-7.5, even more preferably 6.2-7.3, and most preferably 6.3-7.2.

[0389] In another preferred embodiment of the present invention, the packaged heat-treated beverage has a pH in the range of 6.0–7.5, more preferably 6.2–7.5, and most preferably 6.3–7.5.

[0390] In a more preferred embodiment of the present invention, the liquid solution has a pH in the range of 6.0-8.0, more preferably 6.6-7.7, even more preferably 6.7-7.6, and most preferably 6.8-7.5.

[0391] For the production of acidic beverages, an acidic liquid solution is particularly preferred. In some preferred embodiments of the present invention, the liquid solution has a pH in the range of 3.0-5.4, more preferably 3.5-5.0, even more preferably 3.7-4.8, and most preferably 4.0-4.6.

[0392] In a more preferred embodiment of the present invention, the liquid solution has a pH in the range of 3.0-5.4, more preferably 3.0-5.0, even more preferably 3.5-5.0, and most preferably 3.5-4.6.

[0393] In a more preferred embodiment of the present invention, the liquid solution has a pH in the range of 3.0-5.4, more preferably 3.1-5.0, even more preferably 3.2-4.6, and most preferably 3.3-3.8.

[0394] The inventors found that the viscosity contribution of soluble whey protein aggregates becomes less significant below pH 4.0. Therefore, in some preferred embodiments of the invention, the liquid solution has a pH in the range of 3.0-4.0, more preferably 3.0-3.8, and most preferably 3.0-3.6. Preferably, the liquid solution can have a pH in the range of 3.0-4.0, more preferably 3.0-3.8, and most preferably 3.0-3.6; the whey protein nanogel can contribute 50-95% w / w, more preferably 55-85% w / w, and even more preferably 60-75% w / w of the total protein in the liquid solution; and the soluble whey protein aggregate can contribute 5-50% w / w, more preferably 15-45% w / w, and most preferably 25-30% w / w of the total protein in the liquid solution.

[0395] The inventors further found that a high content of whey protein nanogel relative to total protein makes it possible to produce a low-viscosity, high-protein beverage with a pH range of 4.0-5.0, most preferably 4.2-4.8. Thus, in some preferred embodiments of the invention, the liquid solution has a pH in the range of 4.0-5.0, most preferably 4.2-4.8. Preferably, the liquid solution can have a pH in the range of 4.0-5.0, most preferably 4.2-4.8, and the whey protein nanogel can contribute at least 80% w / w, most preferably at least 90% w / w, of the total protein in the liquid solution.

[0396] In general, the pH of a liquid solution can be adjusted using any suitable food acid or food base. Those skilled in the art will recognize suitable means for adjusting the pH. Suitable food bases include sodium carbonate or potassium carbonate, sodium bicarbonate or potassium carbonate, or ammonium hydroxide. Alternatively, KOH or NaOH can be used, for example, to adjust the pH. Suitable food acids include, for example, citric acid, hydrochloric acid, malic acid or tartaric acid, or phosphoric acid.

[0397] In some preferred embodiments of the present invention, the liquid solution has a viscosity of at most 200 cP at a shear rate of 20 °C and 300 s -1 and, more preferably, at most 100 cP at a shear rate of 20 °C and 300 s -1 and, even more preferably, at most 50 cP at a shear rate of 20 °C and 300 s -1 and, most preferably, at most 20 cP at a shear rate of 20 °C and 300 s -1 Lower viscosities are possible and often desirable. Thus, in other preferred embodiments of the present invention, the liquid solution has a viscosity of at most 15 cP at a shear rate of 20 °C and 300 s

[0398] and, more preferably, at most 10 cP at a shear rate of 20 °C and 300 s -1 and, even more preferably, at most 8 cP at a shear rate of 20 °C and 300 s -1 and, most preferably, at most 5 cP at a shear rate of 20 °C and 300 s -1 -1 It is particularly preferred that the liquid solution is sterile.

[0399] The liquid solution of the present invention may contain other major nutrients and material components other than proteins. Embodiments and preferences regarding major nutrients and additional material components, as described in connection with packaged heat-treated beverages, equally apply to the liquid solution, and we refer to those embodiments rather than repeating them here.

[0400]

[0401] In some particularly preferred embodiments of the invention, the liquid solution has the same chemical composition as the packaged heat-treated beverage.

[0402] In other particularly preferred embodiments of the invention, the liquid solution has the same chemical composition as the packaged heat-treated beverage, except for less protein denaturation.

[0403] ​The provision of a liquid solution is particularly preferably comprised of combining a whey protein nanogel composition in powder form as defined herein with water and optionally one or more additional material components.

[0404] The powdered whey protein nanogel composition preferably provides at least 50% w / w, more preferably at least 80% w / w, even more preferably at least 90% w / w, and most preferably all of the whey protein nanogel in the liquid solution.

[0405] The powdered whey protein nanogel composition is more preferably to provide at least 50% w / w, more preferably at least 80% w / w, even more preferably at least 90% w / w, and most preferably all of the protein in the liquid solution.

[0406] In some preferred embodiments of the present invention, the liquid solution has a pH in the range of 3.0-5.4, most preferably 3.5-4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the liquid solution, most preferably in the range of 10-22% w / w relative to the weight of the liquid solution. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 85% w / w, most preferably at least 89% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0407] In another preferred embodiment of the present invention, the liquid solution has a pH in the range of 3.0-5.4, most preferably 3.5-4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the liquid solution, most preferably in the range of 10-22% w / w relative to the weight of the liquid solution. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 10% w / w, most preferably at most 5% w / w, relative to the total protein.

[0408] In some preferred embodiments of the present invention, the liquid solution has a pH in the range of 3.0-5.4, most preferably 3.5-4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the liquid solution, most preferably in the range of 10-22% w / w relative to the weight of the liquid solution. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0409] In another preferred embodiment of the present invention, the liquid solution has a pH in the range of 3.0-5.4, most preferably 3.5-4.6, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the liquid solution, most preferably in the range of 10-22% w / w relative to the weight of the liquid solution. - A total amount of BLG of at least 50% w / w, most preferably at least 55% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 50% w / w, most preferably at least 60% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 10% w / w, most preferably at most 5% w / w, relative to the total protein.

[0410] In some preferred embodiments of the present invention, the liquid solution has a pH in the range of 6.2–7.5, most preferably 6.8–7.5, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the liquid solution, most preferably in the range of 10-22% w / w relative to the weight of the liquid solution. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 85% w / w, most preferably at least 89% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 15% w / w, most preferably at most 11% w / w, relative to the total protein.

[0411] In another preferred embodiment of the present invention, the liquid solution has a pH in the range of 6.2–7.5, most preferably 6.8–7.5, and includes the following: -Total amount of protein in the range of 8-32% w / w relative to the weight of the liquid solution, most preferably in the range of 10-22% w / w relative to the weight of the liquid solution. - A total amount of BLG of at least 90% w / w, most preferably at least 95% w / w, relative to total protein. - A whey protein nanogel in an amount of at least 90% w / w, most preferably at least 95% w / w, relative to the total protein, and -Soluble whey protein aggregates in an amount of at most 10% w / w, most preferably at most 5% w / w, relative to the total protein.

[0412] In some preferred embodiments of the present invention, for example, a liquid solution for preparing a sports drink includes the following: -The total amount of carbohydrates is at most 75%, more preferably at most 40E%, even more preferably at most 10E%, and most preferably at most 5E%, of the total energy content (E) of the liquid solution, and - A total amount of lipids of at most 10E%, more preferably at most 6E%, even more preferably at most 3E%, and most preferably at most 1E%.

[0413] In another preferred embodiment of the present invention, for example, a liquid solution for the preparation of a nutritionally complete beverage includes the following: -Total amount of carbohydrates in the range of 30-60% of the total energy amount of the liquid solution, most preferably in the range of 35-50%. -Total amount of lipids in the range of 20-50% of the total energy amount, more preferably in the range of 25-45%, and most preferably 30-40%.

[0414] The packaging in step 2) may be any suitable packaging technique, and any suitable container may be used to package the liquid solution.

[0415] However, in a preferred embodiment of the invention, the packaging in step 2) is aseptic packaging, i.e., the liquid solution is packaged under sterile conditions. For example, aseptic packaging can be carried out by using an aseptic filling system, which preferably involves filling the liquid solution into one or more aseptic containers.

[0416] Aseptic filling and sealing are particularly preferred when the liquid solution is already sterile before filling, or has a very low microbial content.

[0417] Examples of useful containers include bottles, paper cartons, bricks, and / or bags.

[0418] In some preferred embodiments of the process of the invention, the liquid solution of step 1) is subjected to a heat treatment including at least pasteurization, and then packaged in step 2).

[0419] In another embodiment of the process of the invention, the packaged liquid solution of step 2) is subjected to a heat treatment including at least pasteurization.

[0420] In some preferred embodiments, the heat treatment includes heating the liquid solution to a temperature in the range of 70-80°C.

[0421] In some preferred embodiments of the invention, the heat treatment temperature is in the range of 70-80°C, preferably 70-79°C, more preferably 71-78°C, even more preferably 72-77°C, and most preferably 73-76°C, for example, about 75°C.

[0422] Preferably, the heat treatment period is 1 second to 60 minutes when carried out at temperatures in the range of 70-80 degrees. The maximum exposure time is optimal at the lowest temperature in the temperature range, and vice versa.

[0423] In other preferred embodiments, the heat treatment temperature is 70°C for at least 60 minutes, preferably 75°C for at least 45 minutes, preferably 80°C for at least 30 minutes, preferably 85°C for at least 22 minutes, and preferably 90°C for at least 10 minutes.

[0424] In a particularly preferred embodiment of the invention, the heat treatment is provided at 70-78°C for 1 second to 30 minutes, more preferably at 71-77°C for 1 minute to 25 minutes, and even more preferably at 72-76°C for 2 minutes to 20 minutes.

[0425] In some preferred embodiments of the invention, the heat treatment process includes heating to a temperature of 85°C-95°C for 1 to 30 minutes.

[0426] In some embodiments, particularly with respect to BLG, higher temperatures may also be preferred if unfolding and optionally aggregation are required. For example, the heat treatment temperature may be at least 81°C, preferably at least 91°C, preferably at least 95°C, more preferably at least 100°C, even more preferably at least 120°C, and most preferably at least 140°C.

[0427] In other preferred embodiments of the invention, the heat treatment temperature is preferably at least 95°C, more preferably at least 100°C, even more preferably at least 120°C, and most preferably at least 140°C. For example, the heat treatment temperature is preferably in the range of 95-160°C, more preferably in the range of 100-155°C, even more preferably in the range of 120-153°C, and most preferably in the range of 140-152°C.

[0428] In some preferred embodiments of the invention, the heat treatment is thermal sterilization, preferably including a temperature in the range of 120-155°C for a period sufficient to achieve sterility, typically between 0.3 seconds and 10 minutes, more preferably between 140-155°C for 4-30 seconds.

[0429] The heat treatment may include, for example, a temperature in the range of 90-130°C and a duration in the range of 5 seconds-10 minutes. The heat treatment may include, for example, heating to a temperature in the range of 90-95°C for a duration of 1-10 minutes, for example, heating to approximately 120°C for approximately 20 seconds. Alternatively, the heat treatment may include heating to a temperature in the range of 115-125°C for a duration of 5-30 seconds, for example, heating to approximately 120°C for approximately 20 seconds.

[0430] Alternatively, the heat treatment is preferably a sterile UHT-type treatment, which typically involves a temperature in the range of 135–146°C and a duration in the range of 2–10 seconds.

[0431] Alternatively, and also preferred, the heat treatment may include a temperature in the range of 145-180°C and a duration in the range of 0.01-2 seconds, more preferably a temperature in the range of 150-180°C and a duration in the range of 0.01-0.3 seconds.

[0432] The execution of the heat treatment may include the use of equipment such as plate or tube heat exchangers, scraped surface heat exchangers, or retort systems. Alternatively, particularly preferably for heat treatment above 95°C, direct steam-based heating may be used, for example, direct steam injection, direct steam injection, or spray cooking. In addition, such direct steam-based heating is preferably used in combination with flash cooling. A preferred example of the execution of spray cooking is found in WO2009113858A1 (which is incorporated herein by reference for all purposes). Preferred examples of the execution of direct steam injection and direct steam injection are found in WO2009113858A1 and WO2010 / 085957A3 (which are incorporated herein by reference for all purposes). General embodiments of high-temperature treatment are found, for example, in “Thermal technologies in food processing” ISBN 185573558 X, which is incorporated herein by reference for all purposes.

[0433] In some preferred embodiments of the invention, the heat treatment includes, or further comprises, a retort heat treatment at a temperature of at least 80°C, more preferably at least 95°C, even more preferably at least 100°C, and most preferably at least 120°C. As seen in Example 10, the inventors have demonstrated that the beverage according to the present invention can withstand a retort heat treatment at 150°C for 10 minutes.

[0434] In other preferred embodiments of the invention, the heat treatment includes, or further comprises, steam injection or spray cooking at a temperature of preferably at least 100°C, more preferably at least 120°C, even more preferably at least 130°C, and most preferably at least 140°C.

[0435] In some preferred embodiments of the invention, pasteurization is combined with physical microbial reduction.

[0436] Useful examples of physical microbial reduction include one or more of microbial filtration, UV irradiation, high-pressure treatment, pulsed electric field treatment, and ultrasound.

[0437] In some preferred embodiments of the invention, the heat treatment is a sterilization heat treatment, thus obtaining a sterile liquid solution, and therefore a sterile beverage. Such sterilization can be achieved, for example, by combining microbial filtration and pasteurization, or by carrying out a heat treatment at at least 100°C for a period of time sufficient to achieve sterilization.

[0438] In some particularly preferred embodiments of the invention, the heat treatment includes heating the liquid solution to a temperature in the range of 100–160°C for a period of time sufficient to sterilize the liquid solution. This preferably includes heating the liquid solution to a temperature in the range of 120–155°C for a period of time sufficient to achieve a sterile state, typically 0.3 seconds to 10 minutes, more preferably 140–155°C for 0.3–30 seconds.

[0439] It is beneficial to subject the liquid solution to cooling after heat treatment. According to a preferred embodiment of the process of the invention, following the heat treatment, the heat-treated liquid solution is cooled in an optional step to preferably 0-50°C, preferably 0-25°C, preferably 0-20°C, preferably 0-15°C, preferably 0-10°C, preferably 4-8°C, preferably 2-5°C, and preferably 1-5°C.

[0440] If the liquid solution is at least pasteurized, it is preferably cooled to 0-15°C, more preferably 1-5°C, after heat treatment.

[0441] Cooling can occur before or after the filling step.

[0442] In some preferred embodiments of the invention, packaged heat-treated beverages can be obtained by the above process.

[0443] The food may instead be acidic or concentrated. The inventors have observed that a whey protein nanogel composition containing a substantial amount of soluble whey protein aggregates in addition to whey protein nanogels is thermally stable and can increase in viscosity upon acidification. Such a whey protein nanogel composition is useful in applications where the liquid food base is pasteurized or sterilized at a near-neutral pH and then acidified chemically or by bacteria.

[0444] In relation to the present invention, "concentrated food" is 20°C and 300s -1 It has a viscosity exceeding 200 cP at a shear rate. While the concentrated food is viscous, it may still be a pourable liquid, or it may be a coherent gel.

[0445] In relation to the present invention, "acidic foods" have a pH of at most 5.6 at 25°C.

[0446] Therefore, a particular aspect of the invention relates to a process for producing an acidic, concentrated food product and includes the following steps: - A step of preparing a liquid food base having a pH of at least 5.7, wherein the liquid food base comprises a whey protein nanogel composition sufficient to provide a 4-20% w / w amount of protein, and the whey protein nanogel composition preferably comprises the following steps as specified herein: -Soluble whey protein aggregates in an amount of 15-70% w / w, more preferably 20-50% w / w, relative to total protein. -Whey protein nanogel in an amount of 30-85%, more preferably 50-80% w / w relative to total protein, - A step of heating the liquid food base at at least 70°C for a period of time sufficient to at least pasteurize the liquid food base. -Optionally, a step of homogenizing a heat-treated liquid food base, - A step of acidifying the heat-treated liquid food base to a pH of at most 5.4. -Optional step of homogenizing the acidified food base Acidic, concentrated foods are mixtures of an acidified food base or an acidified liquid food base and further ingredient components such as sweeteners and / or flavorings.

[0447] Another specific aspect of the invention relates to an acidic, thick food product, preferably in the form of a pourable, viscous liquid or a non-pouring gel, which can be obtained by the above process.

[0448] Furthermore, one aspect of the invention relates to the use of whey protein nanogel compositions and / or multiple whey protein nanogels as defined herein for one or more of the following: -As a food ingredient, - As a food ingredient for producing a sterile beverage containing at least 10% w / w protein, more preferably at least 21% w / w protein, pH less than -5.5, and 20°C and 300s -1 As a food ingredient for producing a concentrated food having a viscosity exceeding 200 cP when measured at a shear rate, and -For example, as a whitening agent in coffee cream.

[0449] A further aspect of the invention relates to the use of whey protein nanogels and / or whey protein nanogel compositions as a protein source for reducing the astringency and / or acidity of heat-treated protein beverages having a pH of 3.0-5.0, most preferably 3.5-4.6. - Preferably, the whey protein nanogel provides at least 50% w / w of the total protein of the heat-treated beverage, more preferably at least 70% w / w, even more preferably at least 80% w / w, and most preferably at least 90% w / w of the total protein of the heat-treated beverage; and - Preferably, the heat-treated beverage contains a total protein amount of 2-35% w / w, more preferably 4-30% w / w, even more preferably 6-25% w / w, and most preferably 8-20% w / w.

[0450] Preferably, the whey protein nanogel of the invention contains a total amount of BLG of at least 60% w / w, more preferably at least 70% w / w, even more preferably at least 80% w / w, and most preferably at least 90% w / w.

[0451] The whey protein nanogel and / or whey protein nanogel composition used as described above is preferably a whey protein nanogel and / or whey protein nanogel composition as defined herein, and can preferably be obtained by the method of the present invention.

[0452] The present invention has been described above with reference to specific embodiments. However, other embodiments not described herein may also be within the scope of the invention. Different features and steps of various embodiments and aspects of the invention may be combined in ways other than those described herein unless otherwise specified.

[0453] Examples Method of Analysis Analysis 1: Determination of aggregate morphology by transmission electron microscopy. The sample was fixed in 2% glutaraldehyde phosphate buffer (pH 7.2) at a 1:1 volume ratio for 40 minutes at room temperature. The fixed sample was then diluted in water to a protein concentration of approximately 0.2%. 4 μl of the diluted sample was placed on a discharged Formvar / carbon film grid (300 mesh) for 1 minute, followed by blotting with filter paper. Staining was performed by adding 4 μl of phosphotungstic acid (1%, pH 7.0) for 1 minute, followed by blotting. The grid was washed once with MilliQ water, dried, and then inserted into a Philips CM-100 electron microscope operating at 100 kV. Images were obtained at at least five different locations on the grid.

[0454] Analysis 2: Determination of aggregate size by dynamic light scattering The hydrodynamic diameter of the whey protein nanogel was measured using a Malvern Nanosizer S instrument. A whey protein nanogel preparation diluted to a protein concentration of 0.05% or less in milliQ water was placed in a 2.5 mL disposable cuvette measuring 12.5 x 12.5 x 45 mm, with the arrow marker indicating the direction of the instrument laser. The sample was measured at 20 °C after a 30-second equilibration time with automatic adjustment of the attenuation rate and measurement period determined by the software. The average Z-average hydrodynamic diameter in nanometers from five measurements provided by the software is presented.

[0455] Analysis 3: Quantification of the amounts of whey protein nanogel, soluble whey protein aggregates, microparticles, and residual protein The amounts of whey protein nanogel, whey protein microparticles, soluble whey protein aggregates, and residual protein were determined by fractionation of the sample (diluted to 4% protein in milliQ water (18.2 MΩ) and adjusted to pH 7.0) as described below. The protein content of each fraction was determined as described in Analysis 7.

[0456] The amount of microparticles was determined by filtering a 5.0 mL subsample of the 4% protein solution through a 2.0 μm syringe filter and measuring the difference between the total amount of protein in the initial subsample (P total ) and the total amount of protein in the filtrate (P filtrate ). The amount of whey protein microparticles relative to the total protein was calculated as follows:

Equation

[0457] Therefore, a solution of the sample containing 4.0% (w / w) total protein and having a pH of 4.6 was prepared by pH adjustment using 5% (w / w) HCl(aq). The solution was stored at room temperature for 2 hours, and then centrifuged at 50,000 g for 1 hour. The total amount of protein in the supernatant was measured.

number

number

number

[0458] Therefore, a subsample of 4.0% protein solution (pH 7.0) was stored at room temperature for 2 hours, and then centrifuged at 50,000 g for 1 hour. Total amount of protein in the supernatant.

number

number

[0459] The amount of soluble whey protein aggregates relative to total protein was determined as follows:

number

[0460] The degree of protein denaturation was determined as 100% minus residual protein (%).

[0461] Analysis 4: Viscosity of the liquid sample Viscosity was measured at 20°C using a handheld capillary viscometer (Viscoman, Gilson) and measured over 300 seconds. -1 The shear rate was reported.

[0462] Analysis 5: Quantification of gel formation during acidification Gel formation and viscosity development of samples containing whey protein nanogels during acidification were evaluated using a rheometer (Anton Paar Physica MCR301). The whey protein nanogel samples were diluted with desalted water to a total protein content of 4 w / w% and equilibrated at 42°C for 10 minutes. GDL (D-gluconate δ-lactone) was added from powder form to the stirred solution to a final concentration of 1 w / w% and dissolved under stirring for 1 minute.

[0463] 20 mL of the solution was added to a cup (CC27-SS) in a rheometer pre-equilibrated to 42°C, and the storage and loss modulus were measured at 0.1 Hz and 0.5% tensile strength for 60 minutes. pH was recorded throughout the experiment using a WTW Multi 3410 pH logger calibrated with standard solutions at 42°C.

[0464] Analysis 6: Determination of natural BLG, natural ALA, and CMP, and determination of the degree of BLG denaturation. Protein samples (unheated and heated) were diluted in 2% MQ water. 5 mL of the protein solution, 10 mL of Milli-Q, 4 mL of 10% acetic acid, and 6 mL of 1.0 M NaOAc were mixed and stirred for 20 minutes to precipitate and aggregate denatured proteins at approximately pH 4.6. The solution was filtered through a 0.22 μm filter to remove aggregates and non-native proteins. All samples were subjected to the same dilution by adding polished water. For each sample, the same volume was subjected to a ULC column.

number

[0465] The sample was run under the following conditions: Buffer A: Milli-Q water, 0.1% w / w TFA Buffer B: HPLC-grade acetonitrile, 0.1% w / w TFA Flow rate: 0.4ml / min Gradient: 0-6.00 min 24-45%B; 6.00-6.50 min 45-90%B; 6.50-7.00 min 90%B; 7.00-7.50 min 90-24%B and 7.50-10.00 min 24%B.

[0466] The concentration of native BLG in the sample was determined using the area of ​​the BLG peak relative to the protein standard (Sigma L0130) (5-level calibration curve). The sample was further diluted and reinjected if it fell outside the linear range. The degree of BLG denaturation (D) provided by heat treatment was calculated as follows: D=((BLG native,non-heated -BLG native,heated ) / BLG native,non-heated ) * 100%.

[0467] Analysis 6 is also used to determine the content of natural BLG, natural ALA, and CMP in the sample.

[0468] Analysis 7: Determination of total protein The total protein content (true protein) of the sample is determined as follows: 1) Determine the total nitrogen of the sample using the Kjeldahl method, in accordance with ISO8968-1 / 2|IDF020-1 / 2-Milk-Determination of Nitrogen Content-Part 1 / 2:Determination of Nitrogen Content. 2) Determine the non-protein nitrogen content of the sample in accordance with ISO8968-4|IDF020-4 - Milk - Determination of nitrogen content - Part 4: Determination of non-protein nitrogen content. 3) Total protein (m total nitrogen -m non-protein-nitrogen ) * Calculate using 6.38.

[0469] Analysis 8: Determination of total lipid content The amount of lipids is determined according to ISO 1211:2010 (Determination of fat content - Rose-Gottlieb gravimetric method).

[0470] Analysis 9: Determination of the total amount of lactose The total amount of lactose is determined according to ISO 5765-2:2002 (IDF 79-2:2002) "Powdered milk, dry ice mixtures and processed cheeses - Determination of lactose content - Part 2: Enzymatic method utilizing the galactose portion of lactose".

[0471] Analysis 10: Brix's Decision Brix measurements were performed using an Atago PAL-α digital handheld refractometer calibrated to polished water (water filtered by reverse osmosis to obtain a conductivity of at most 0.05 mS / cm).

[0472] Approximately 500 μl of the sample was transferred to the prism surface of the instrument, and the measurement was started. The measured values ​​were read and recorded.

[0473] The Brix value of whey protein solution is proportional to the total solids (TS) content, and TS (measured in %w / w) is approximately equal to Brix. * It is 0.85.

[0474] Analysis 11: Determination of Ash Content The ash content of food is determined according to NMKL173:2005, "Determination of Ash Content in Food by Gravimetric Measurement."

[0475] Analysis 12: Determination of total solids and water content The total solids of the product may be determined according to NMKL 110, 2nd edition, 2005 (Total Solids (Water) - Gravimetric Determination in Milk and Dairy Products). NMKL is an abbreviation for "Nordisk Metodikkomite for Naringsmidler".

[0476] The water content of a product can be calculated as 100% - relative amount of total solids (%w / w).

[0477] Analysis 13: pH measurement All pH values ​​are measured at 25°C using a pH glass electrode. The pH glass electrode (with temperature compensation) should be carefully rinsed and calibrated before use. If the sample is in liquid form, the pH is measured directly in the liquid solution at 25°C. If the sample is in powder form, dissolve 10 grams of powder in 90 ml of desalinated water at room temperature with vigorous stirring. Then, measure the pH of the solution at 25°C.

[0478] Analysis 14: Determination of calcium, magnesium, sodium, potassium, and phosphorus levels (ICP-MS method) The total amounts of calcium, magnesium, sodium, potassium, and phosphorus are determined using a procedure in which the sample is first decomposed using microwave decomposition, and then the total amount of minerals is determined using an ICP instrument.

[0479] Device: The microwave source is Anton Paar, and the ICP is an Optima 2000DV manufactured by PerkinElmer Inc. material: 1M HNO3 Yttrium in 2% HNO3 Suitable standards for calcium, magnesium, sodium, potassium, and phosphorus in 5% HNO3 Pre-processing: A certain amount of powder is weighed out and transferred to a microwave decomposition tube. 5 mL of 1 M HNO3 is added. The sample is decomposed in the microwave according to the microwave usage instructions. The decomposed tube is placed in a ventilation chamber, the lid is removed, and the volatile fumes are evaporated. Measurement procedure: The pre-treated sample is transferred to the DigiTUBE using a known volume of Milli-Q water. A 2% HNO3 solution containing yttrium is added to the decomposition tube (approximately 0.25 mL per 50 mL of diluted sample), and diluted with Milli-Q water to a known volume. The sample is analyzed by ICP using the procedure described by the manufacturer.

[0480] A blind sample is prepared by diluting a mixture of 10 mL of 1 M HNO3 and 0.5 mL of a 2% HNO3 solution containing yttrium using Milli-Q water to a final volume of 100 mL. At least three standard samples are prepared with concentrations that encompass the predicted sample concentration.

[0481] Analysis 16: Determination of thermal solidification time The thermal stability of whey protein is particularly important for high-protein beverages in a neutral pH range, where ultra-high temperature processing is necessary to ensure the long shelf life of the beverage composition.

[0482] Therefore, thermal coagulation time analysis was developed as a measure of thermal stability. A 1.0 mL whey protein nanogel preparation was transferred to a 2 mL 32 × 11.5 mm injection vial (Mikrolab, catalog number ML33003V) and crimped and sealed. The sample was then heated by incubation in an aluminum block preheated to 150°C in a Mikrolab hyperthermal heating unit. The aluminum block had a hole drilled to precisely fit the dimensions of the vial, ensuring efficient heat transfer. A temperature increase of 20–100°C was achieved in 40 seconds, and a temperature of 140°C was reached within 132 seconds.

[0483] Aliquots of individual samples were incubated for (minutes:seconds) 0:45, 1:00, 1:20, 1:47, 2:22, 3:10, 4:13, 5:38, 7:30, or 10:00. The measured temperature inside the sample exceeded 140°C after 132 seconds (2:12), simulating UHT conditions. After heating, the sample was immediately transferred to cold water to stop further reaction. The sample was inverted, and its ability to flow to the bottom was recorded at each heating time. The thermal solidification time (HCT) was determined as the first heating time at which the sample gelled and therefore did not flow to the bottom of the vial when inverted.

[0484] The temperature was recorded by placing a thermocouple thermometer, connected to an Omega HH802 digital thermometer, into a vial containing 1 mL of oil to avoid boiling and evaporation of the sample at high temperatures.

[0485] Analysis 17: Determination of total amounts of BLG and ALA The total amount of BLG and ALA in the sample (including aggregated BLG and / or ALA) is determined according to Example 1.31 of PCT application PCT / EP2019 / 067039.

[0486] Example 1: Preparation of concentrated whey protein nanogel solution The inventors previously discovered, by chance, that whey protein nanogels can be produced in solutions with surprisingly high protein content. The purpose of this embodiment was to further explore the possibility of producing whey protein nanogels at high protein concentrations and to characterize the resulting whey protein nanogel composition.

[0487] material and method: [Table 1] An exemplary whey protein solution was prepared by dissolving BLG isolate powder, which was generated as described in WO2018 / 115520, Example 7. The properties of the BLG isolate powder are shown in Table 1.

[0488] Mineral content was determined by analysis 14, and fat, lactose, ash, total solids, and total protein were determined by analyses 8, 9, 10, 11, 12, and 7, respectively. Protein composition was determined using analysis 6.

[0489] The powder was weighed out, and considering the protein / total solids, final whey protein compositions with 4%, 8%, 10%, 12%, and 16% protein were prepared. 90% milli-Q water was added to the samples, and the pH was adjusted to 5.9 (or pH 6.0 for 10% protein) using 3M NaOH.

[0490] The remaining water was added, and the final pH was checked. 15 mL of each sample in a Duran GL18 threaded tube (wall thickness 1.8 mm, outer diameter 16 mm, catalog number 28625320) with a PBT screw cap (Duran) was heat-treated in a water bath at 90°C for 14 minutes (or 10 minutes with 10% protein), and then immediately cooled in an ice bath.

[0491] Characterization of soluble whey protein aggregates and whey protein nanogels by dynamic light scattering (Z-mean hydrodynamic diameter), transmission electron microscopy, and fractionation was performed as described in analyses 1, 2, and 3, respectively.

[0492] result: Whey protein nanogel preparations were formed by heat treatment with BLG at 90°C for 14 minutes. Surprisingly, the whey nanogel preparations remained liquid even when heated at high protein concentrations of at least 16% protein, as shown in Table 2.

[0493] For example, it has generally been found that heat treatment at 90°C for 10 minutes induces 95-97% denaturation, with only 3-5% of the protein remaining undenatured (according to Analysis 6) after the heat treatment.

[0494] The whey nanogel preparations were characterized by having a z-average diameter of 196–287 nm and, at increased protein concentrations, a fraction of 6–20% soluble whey protein aggregates and a nanogel fraction of 94–80%, respectively (see Figure 1).

[0495] Figure 2 shows a transmission electron microscope image containing highly uniform, spherical nanogels whose individual sizes closely match those of dynamic light scattering measurements (Table 2). During TEM sample preparation, both staining and drying have an effect on the particles, causing them to form clusters together, as shown in Figure 2.

[0496] Non-spherical aggregates are visually abundant in TEM images of 12-16% whey protein nanogel preparations, but spherical aggregates account for >80% of the mass fraction due to their compact structure.

[0497] Further findings indicate that the increase in the fraction of soluble aggregates with increasing protein concentration coincided with the appearance of smaller, chain-like aggregates in TEM images, suggesting that increased protein concentration and / or increased Na and K content result in an increase in the fraction of soluble aggregates. [Table 2]

[0498] Conclusion: Whey protein nanogel preparations can be prepared even at protein concentrations of up to 16% when using a whey protein solution characterized by low calcium (0.0016Ca:BLGw:w) and monovalent salts. The resulting whey protein nanogel preparations consist mostly (≧80%) of spherical nanogels having a size of 211-287 nm, with a small fraction of soluble whey protein aggregates.

[0499] The fraction of soluble whey protein aggregates increases with increasing protein and / or monovalent salt content (Na+K).

[0500] Example 2: Whey protein nanogel preparation having a low content of soluble aggregates The objective of this whey protein nanogel preparation is to demonstrate how monovalent and divalent cations present during the heat treatment of a whey protein composition affect the distribution between the nanogel and soluble whey protein aggregates, ultimately enabling heat treatment of whey protein solutions at high protein concentrations without gelation, thereby forming whey protein nanogels.

[0501] material and method: Whey protein nanogel preparations were prepared by weighing out BLG powder from the BLG powder used in Example 1, which had the composition described in Table 1, to reach 3%, 4%, 5%, and 16% BLG (all with a calcium content of 0.0016 g per gram of BLG). The powder was dispersed in Milli-Q water to the desired concentration, dissolved by adjusting the pH to 6.0 using 3M NaOH, and the amount of added minerals was recorded. 0-50 mM NaCl was added to the preparation from the 1M stock solution. The total molar concentration of Na+K was calculated by summing the intrinsic content of Na+K in the powder using their individual molecular weights, the amount of Na added in the form of NaCl, and the total amount of Na+K obtained, and is shown in Table 3.

[0502] Each 1 mL sample in a 2 mL clear, crimp-sealed vial (Agilent Technologies, Germany) was heated for 10 minutes in an aluminum block preheated to 90°C. The size of the whey protein nanogel was evaluated by light scattering analysis 2, the flow behavior (gel / liquid) was evaluated by assessing the sample flow to the bottom upon sample inversion, and the sample viscosity was measured using Viscoman as described in analysis 4.

[0503] Sample AE was prepared from the same BLG powder to create a 12% BLG composition with an intrinsic Ca content of 0.0016 g / g BLG. The BLG powder was weighed out, dispersed in MilliQ water, and dissolved by adding 3M NaOH to reach a pH of 5.9 (Sample A).

[0504] The sample BE was prepared by further titration with 3M NaOH to reach pH 6.0, 6.1, 6.3, and 6.5, respectively.

[0505] Each 15 mL sample (AE) was heated at 95°C for 15 minutes by immersion in a water bath in a Duran glass tube, and immediately after heating, it was cooled in an ice bath.

[0506] Sample FL was prepared from the same BLG powder, and a 14% BLG solution with a calcium content of 0.0021 g / g BLG was prepared. The BLG powder was weighed out, dispersed in Milli-Q water, and dissolved by titration to a Ca content of 0.0021 g / g BLG and a pH of 5.97 using a 5% Ca(OH)2 slurry (stirred to ensure homogeneity) (Sample F). Sample GK was prepared from Sample F by adjusting the pH to 6.1-6.7 using 3M NaOH (see table), and the amount of NaOH added during this process was recorded.

[0507] Each 15 mL of sample FL was heated in a water bath at 95°C for 14 minutes to prepare whey protein nanogels, which were then cooled immediately after heating.

[0508] Sample set M was prepared as described for sample FL. After initial pH adjustment to 5.97 using 1M CaCl2 to 7.5mM CaCl2, the calcium content was reached at 0.0044 g / g BLG. The pH was adjusted to 5.9-6.5 using 3M NaOH, and the sample was heated as described for sample FL.

[0509] Sample set N was prepared as described for sample set M, but the Ca content was increased to 0.0065 g / g BLG by adding 14.9 mM CaCl2. Aliquots of the sample were adjusted to a pH in the range of 5.9–6.7 using 3 M NaOH and heated as described for sample FL.

[0510] Additional whey protein nanogel preparations (OPQ) were prepared by dissolving BLG powder using a 5% Ca(OH)2 slurry to pH levels of 6.04-5.94-5.89, reaching 14-16-20% BLG, and achieving Ca content of 0.0022, 0.0024, and 0.0023 g / g BLG, respectively. The pH was then adjusted using 3M NaOH to pH levels of 6.11, 6.10, and 6.08, respectively. Whey protein nanogel preparations (OPQ) with a low content of soluble whey protein aggregates were then prepared by heating a 15 mL sample in a Duran glass tube in a 95°C water bath for 14 minutes. The viscosity of the sample OPQ was determined according to Analysis 4.

[0511] Samples R and S were prepared as described for sample F, and then titrated to pH 6.2 and 6.4, respectively, using 5% Ca(OH)2, and heated as described for sample FL. The calcium content of the samples was 0.0028 and 0.0030 g / g BLG, as shown in Table 4.

[0512] The Z-average size and the distribution between nanogels and soluble whey protein aggregates in the whey protein nanogel preparation were characterized by analyses 2 and 3, respectively. Viscosity was determined by analysis 4, and mineral content was determined as described in analysis 14.

[0513] result: A 1.0 mL whey protein composition characterized by an intrinsic calcium content of 0.0016 g / g BLG was adjusted to pH 6.0, 0-50 mM NaCl was added, and the mixture was heat-treated in an aluminum block at 90°C for 10 minutes. The amount of NaCl added after adjustment and the total amount of Na+K obtained can be seen in Table 3 (3%, 4%, and 5% whey protein solutions) and Table 4 (16% whey protein solution).

[0514] While we have demonstrated that whey protein nanogel preparations can be formed even with natural BLG up to at least 16% (Example 1), the inventors found it quite surprising that the apparent threshold concentration is approximately 20 mM total Na+K. Beyond this, the whey protein solution forms a gel upon heat treatment. At lower protein concentrations (3-5%), whey protein nanogel preparations can finally be formed down to 23-25 ​​mM total Na+K.

[0515] Beyond this approximate monovalent mineral content, heat treatment results in gelation of the sample, regardless of whether the protein dosage is 3%, 4%, 5% (Table 3), or even 16% protein (Table 4). In contrast, all samples containing <20 mM Na+K (16%) or <25 mM (3-5%) remain liquid, thus clearly demonstrating the feasibility of producing whey protein nanogel preparations with low monovalent mineral content. Table 4 further reveals that even a slight increase in total Na+K from 15.2 to 19.5 increases the viscosity of a 16% whey protein solution from 24 cP to >100 cP upon heat treatment. [Table 3] [Table 4]

[0516] To minimize the addition of monovalent minerals, the use of Ca(OH)2 slurry was employed, thereby attempting to adjust the pH of the 14% whey protein composition by adding divalent cations instead of monovalent cations during titration.

[0517] Therefore, a 14% whey protein composition was prepared by dissolving BLG using a pH adjustment solution of Ca(OH)2 to pH 5.97, resulting in a Ca content of 0.0021 g / g BLG. However, as shown in Table 6 (Sample FL), heat treatment at 95°C for 10 minutes resulted in gelation of the sample.

[0518] Therefore, the pH was further increased by using 3M NaOH, the calcium content was kept constant at 0.0021 g / g BLG, and the electrostatic repulsion between proteins was increased during this process. Surprisingly, this allowed for the formation of whey protein nanogel preparations with 14% protein at a pH of at most 6.1, and at least 6.7, by heat treatment at 95°C for 10 minutes. As shown in Table 6, the total Na+K remained ≤20 mM within this pH range.

[0519] Surprisingly, the fraction of soluble aggregates in the heated whey protein nanogel preparation remained remarkably low (≤2%) at pH 6.1–6.3, and there was no sign of precipitation in the sample regardless of the high protein concentration used, making it particularly beneficial to prepare the nanogels within this pH range.

[0520] Even more surprisingly, it was found that a calcium content of approximately 0.0022–0.0024 (sample OPQ) g / g BLG, achieved by a two-step pH adjustment (1) using Ca(OH)2 to reach the desired calcium content, and (2) increasing the pH to approximately 6.1 to ensure that the total Na+K was well below 20 mM, allowed for heat treatment of protein concentrations up to at least 20% BLG, as shown in Table 6.

[0521] However, if the calcium content is not altered by the addition of CaCl2, Ca(OH)2, or other sources, it is demonstrated that in 12% whey protein nanogel preparations heat-treated at pH 5.9–6.1 as shown in Table 6 (Sample AD, 0.0016 g / g BLG), the fraction of soluble whey protein increases significantly with pH, ​​ultimately leading to gelation at pH ≥ 6.3.

[0522] Table 6 (Sample Set MN) further demonstrates that when CaCl2 is added, increasing the calcium content in the whey protein composition from 0.0043 to 0.0065 g / g BLG at a pH in the range of 5.9-6.7, gelation occurs upon heat treatment.

[0523] Surprisingly, even when the pH was increased solely by using Ca(OH)2, and liquid whey protein nanogel samples R and S were prepared by heat treatment at 94°C for 14 minutes at pH 6.2–6.48, respectively, nanogel formation was achievable with 0.0028–0.0030 g calcium / g BLG and 3.7 mM total Na+K (see Table 6). [Table 5] [Table 6]

[0524] Conclusion: Whey protein nanogel preparations containing at least 98% nanogel were successfully prepared by controlling the calcium / BLG ratio and pH while maintaining a low monovalent mineral content (≤20 mM total Na+K). Suitable calcium content and total Na+K levels were achieved by combining suitable protein raw materials with pH adjustment using Ca(OH)2 and NaOH to reach appropriate mineral levels.

[0525] Aggregate sizes were observed in the 276–563 nm range at a nanogel content of ≥90%. It was observed that a higher pH is required for nanogel formation to avoid gelation in the presence of higher calcium levels, while excessively high pH levels also result in gelation due to the formation of large fractions of soluble whey protein aggregates. Therefore, an intermediate pH value tailored to a specific calcium content is required for optimal performance.

[0526] Example 3: Whey protein nanogel prepared at high temperature Whey protein solutions containing 4-16% BLG were heat-treated at temperatures ranging from 85 to 150°C to evaluate the opportunity for whey protein nanogel formation over a wide temperature range.

[0527] material and method: The solution was prepared by dissolving BLG as described in Example 1 by adjusting the pH of the whey protein solution to 5.9 with 3M NaOH.

[0528] Sample set A was heat-treated at 85°C for 22 minutes. 120 μl each of 4-16% BLG solution, pH 5.9, was transferred to a 96-well PCR plate (VWR, catalog no. 732-2387) and sealed with adhesive aluminum foil (VWR catalog no. 60941-126). The plate was heated in an Esco Healthcare Swiftmax MaxPro thermal cycler programmed to equilibrate the sample at 20°C for 5 minutes, then heat to the target temperature at 4°C / second, and maintain at the target temperature of 85°C for the specified period of 22 minutes. The sample was then cooled to 4°C.

[0529] Sample set B was identical to sample set A, but it was heat-treated at a higher temperature of 95°C for 14 minutes to produce a whey protein nanogel preparation.

[0530] Sample set C was prepared as described above and consisted of a 12% BLG solution whose pH was adjusted to the range of 5.9–6.0 and 6.1 using 3M NaOH. 10 mL of the 12% BLG solution at each pH was heated in a water bath at 95°C for 10 minutes, as described in Example 1.

[0531] Sample set D consisted of a 12% BLG solution at pH 5.9–6.0, prepared as described for sample set C. However, sample set D was heat-treated by incubation at 150°C for 0–10 minutes. 1.0 mL of the sample was transferred to a 2 mL 32 × 11.5 mm injection vial (Mikrolab, catalog number ML33003V) and crimped and sealed. The sample was then heated by incubation in an aluminum block preheated to 150°C in a Mikrolab superheating unit. The aluminum block had a hole drilled to precisely fit the dimensions of the vial, ensuring efficient heat transfer. Aliquots of individual samples were incubated for typically (minutes:seconds) 0:45, 1:00, 1:20, 1:47, 2:22, 3:10, 4:13, 5:38, or 7:30, and the temperature within the samples, measured to simulate UHT conditions, exceeded 140°C after 132 seconds (2:12). After heating, the samples were immediately transferred to cold water to stop further reactions.

[0532] Sample E was prepared as a 14% BLG solution as described in Sample Set FL in Example 2, and its pH was adjusted to 6.2 using 3M NaOH.

[0533] The Z-average size of the whey protein nanogel preparations was determined as described in Analysis 2. Mineral content was determined using Analysis 14. The thermal solidification time and distribution between nanogels and soluble whey protein aggregates were determined using Analysis 16 and 3, respectively.

[0534] result: Table 7 highlights that whey protein nanogels, characterized by Na and K concentrations concentrated between 3.8 and 16 mM and a Z-average diameter of approximately 180-390 nm, can be prepared by heating a protein solution with a calcium content of at most 4% to at least 12% and a temperature range of at most 85°C to at least 95°C, at a pH of approximately 6.

[0535] Furthermore, when a 14% natural whey protein composition characterized by 0.0022 g calcium / g BLG and Na+K aggregated to 6.9 mM was heat-treated by incubation in a 150°C heat block for 0-7:30 minutes, surprisingly, the resulting nanogel preparation remained liquid even after heat treatment at 150°C for at least 5:38-7:30 minutes at pH 6.0 and 5.9, respectively, and was found to flow freely to the bottom of the HPLC vial when inverted. [Table 7] [Table 8]

[0536] Conclusion: It was found that whey protein nanogel preparations can be prepared at a surprisingly wide temperature range, for example, 85°C for 22 minutes or 150°C for 7:30 minutes, and at remarkably high BLG concentrations ranging from at most 4% to at least 16% protein.

[0537] Since 140°C is reached after 2 minutes and 12 seconds of heating in a 150°C heat block, an astonishingly long effective holding time of over 4 minutes and 30 seconds is achieved, and as a result, a high thermal load of 12-14% can be applied to the sample, during which time a whey protein nanogel in liquid form is still produced.

[0538] It is generally believed that heating high-protein concentrates under UHT conditions without shearing will cause gelation and instrument blocking. Therefore, surprisingly, it was found that treatment with 12-14% natural BLG under UHT conditions did not cause gelation of the sample even without the application of shearing force. This is particularly surprising, as BLG is considered to be one of the least thermally stable whey proteins.

[0539] The obtained nanogel size of approximately 184–389 nm is in good agreement with the aggregate size observed by TEM in the previous example and in Figure 2.

[0540] Example 4: Thermally stable whey protein nanogel preparation This study aims to demonstrate that protein nanogel preparations are suitable for use in ultra-high temperature processing and are ideal for use in high-protein beverages with a neutral pH.

[0541] material and method: The 14-16-20% whey protein nanogel preparation was as described for sample OPQ in Example 2.

[0542] The 14-16 and 20% nanogel preparations were subjected to a second heat treatment at UHT temperature to evaluate their thermal stability, which is defined by the first heating time during which the sample solidifies. This time is called the thermal solidification time and is measured according to Analysis 16.

[0543] Furthermore, the 14% sample was concentrated to 24% protein by ultrafiltration as follows: A 150 mL whey protein nanogel preparation was concentrated by placing it in a 200 mL Amicon stirred cell equipped with a Koch HFK 328 membrane having a nominal molecular weight cutoff of 5 kDa. The sample was concentrated by applying 3 bar N2 gas to pressurize the cell and forcing the liquid through the ultrafiltration membrane. The Brix of the residue and filtrate was measured, and the residue protein content was calculated as described in Analysis 10. During concentration, the pressure was temporarily released, and the top of the cell was removed to allow measurement of protein concentration by Brix (Analysis 10) and viscosity as described in Analysis 4.

[0544] The thermal coagulation time of the 24% concentrate was determined according to Analysis 16.

[0545] The Z-mean diameter and viscosity of the whey protein nanogel preparations were determined by analyses 2 and 4, respectively. The distribution between whey protein nanogels and soluble whey protein aggregates was determined using analysis 3.

[0546] result: Table 9 summarizes the properties of whey protein nanogel preparations produced by heat treatment of high-protein concentrates.

[0547] The unheated solutions were characterized by their low monovalent ion content, indicated by 0.0022–0.0024 gCa / gBLG and a total Na+K of less than 11 mM.

[0548] Whey protein nanogel preparations were characterized by surprisingly low viscosities of 2.9–4.7 cP despite high protein content (14–20%, respectively), and the Z-mean diameter of aggregates was found to be in the range of approximately 350–560 nm. Remarkably high nanogel content (>98%) relative to total protein was found in the samples.

[0549] As shown in Table 9, surprisingly, the nanogel preparations were found to be particularly thermally stable. This is because all samples with 14%, 16%, and 20% protein, and even the 14% whey protein nanogel preparation concentrated to 24%, remained liquid after 2 minutes and 20 seconds of heating. Therefore, to resist UHT temperatures and promote gelation, further heating at 150°C was required for at least 7 minutes and 30 seconds for the 14-16% preparations, or 3 minutes and 10 seconds for the 20% and 24% protein preparations. See Table 9. [Table 9]

[0550] Conclusion: Thermally stable whey protein nanogel preparations with a diameter of approximately 353–562 nm and low viscosity can be prepared at high protein concentrations by heat treatment with pH 14–20% protein, 0.0022–0.0024 g calcium / g BLG, and less than 10.6 mM Na+K. Samples were characterized by a high fraction (>98%) of whey protein nanogels and found to be remarkably resistant to heat treatment. This is because they remained liquid even after heat treatment exceeding 140°C, and even a 14% sample concentrated to 24% protein by ultrafiltration resisted heating up to UHT temperatures.

[0551] Example 5: Low-viscosity whey protein preparation We evaluated the feasibility of producing whey protein nanogel preparations with a low content of soluble aggregates, thereby reducing the protein contribution of soluble whey protein aggregates and manufacturing highly concentrated whey protein nanogel preparations.

[0552] Low viscosity high protein offers a strong advantage in industrial processes where the ability to reach higher protein concentrations directly increases the capacity of the spray dryer. Low viscosity progression is even more desirable in production because the flux across the membrane (e.g., in the context of ultrafiltration) increases inversely proportional to the viscosity of the liquid being filtered.

[0553] Low viscosity is even more desirable in high-protein whey protein beverages and high-protein yogurts.

[0554] material and method: 200 mL of 14% BLG composition was prepared by dispersing the powder in MilliQ, adjusting the pH to 6.0 using a 5% Ca(OH)2 slurry, and then making a final pH adjustment to 6.2 using 3M NaOH. The sample was divided into several 15 mL aliquots, immersed in a 95°C water bath for 14 minutes, heated, and immediately cooled to pool into a single sample.

[0555] The samples were concentrated by UF enrichment, and the protein concentration and viscosity were monitored at appropriate time points during this process.

[0556] The viscosity of the whey protein nanogel preparation was measured using a rheometer (Anton Paar, Physica MCR301). 19.6 mL of the sample was added to cup CC27-SS (SN33864), and the sample was equilibrated at 8°C. 1 s -1 and 1000s -1 A shear rate sweep was performed over 10.5 minutes. Viscosity was measured in centipoise (cP) for 300 seconds. -1 The values ​​were presented in terms of shear rate.

[0557] UF concentration was performed by placing 150 mL of 14% sample in a 200 mL Amicon stirred cell fitted with a Kock HFK328 membrane. The cell was pressurized by applying 3 bar of N2 gas and the sample was concentrated. The Brix of the filtrate was consistently measured at 0.0, thus equivalent to water and suggesting no protein passage through the membrane. During concentration, the pressure was temporarily released to allow for measurement of protein concentration by Brix as described in Analysis 10 and viscosity as described in Analysis 4. After concentration to 24% protein, the sample was removed and left overnight at 4°C.

[0558] result: Table 10 describes the properties of nanogel preparations containing 95.5% nanogel prepared by heat treatment of 14% protein at 95°C for 14 minutes with a calcium content of 0.0022 g / g BLG in the presence of Na and K at a combined concentration of 6.9 mM. While such heat treatment of concentrated whey protein preparations typically results in gelation and / or requires high shear, for example, by using a scraping heat exchanger, to avoid gelation during heating, the inventors found that the heat-treated whey protein preparations remained remarkably low viscosity, comparable to the natural whey protein solution within experimental error, as shown in Table 10.

[0559] The whey protein nanogel preparations were further concentrated by ultrafiltration, during which the viscosity progression was monitored as a function of protein content, as shown in Figure 3. Surprisingly, the nanogel preparations could be concentrated to at least 29.5% protein, and the viscosity, contrary to expectations, consistently followed the viscosity of the unheated whey protein solution up to at least 29.5% protein. [Table 10]

[0560] Conclusion: The combination of high protein (14%), low Na+K, and 0.0022 g calcium / g BLG, along with heat treatment at 95°C for 14 minutes, produced a stable whey protein nanogel preparation characterized by 95.5% nanogel relative to total protein and a Z-average size of 305.5 ± 2.8 nm. Even the viscosity of the concentrated whey protein nanogel preparation was consistently low, found to be approximately equal to that of the natural BLG solution, even when concentrated to high protein levels of at least 29.5%.

[0561] This enables the concentration of whey protein nanogels that are resistant to UHT temperatures (24% in the previous example), making UHT treatment particularly useful at a neutral pH, for example, for medical beverages where high protein content is desirable for certain patient groups.

[0562] Example 6: Low-viscosity acidified product We demonstrated that it is possible to prepare low-viscosity acidified products by generating nanogel preparations containing low amounts of soluble aggregates.

[0563] method: Sample AC was prepared from BLG powder to produce a 12% BLG composition with an intrinsic calcium content of 0.0016 g / g BLG. BLG powder was weighed out, dispersed in MilliQ water, and dissolved by adding 3M NaOH to reach a pH of 5.9 (Sample A). Samples BC were further titrated with 3M NaOH to reach pH 6.0 and 6.2, respectively.

[0564] Sample D was prepared from BLG powder to produce a 16% BLG whey protein nanogel preparation with a particularly low acid-gellable protein content. The protein was weighed out, dispersed in Milli-Q water, and dissolved by titration using a 5% Ca(OH)2 slurry to a pH of 5.94. The pH was then adjusted to 6.0 using 3M NaOH.

[0565] Each 3 × 18 mL sample AD was heated in a Duran glass tube by immersion in a water bath at 95°C for 15 minutes, and immediately after heating, it was cooled in an ice bath.

[0566] Each of the 15-gram samples A and D was weighed out, and either 30 grams of MilliQ (sample AC) or 45 mL of MilliQ (sample D) was added to dilute the samples to 4% protein. The diluted samples were evaluated for gel formation under acidification according to Analysis 5.

[0567] The mineral composition of the whey protein solution was determined using Analysis 14. The distribution between whey protein nanogels and soluble whey protein aggregates was determined using Analysis 3. Structure formation during acidification was determined using Analysis 5.

[0568] result: 12-16% whey protein nanogel preparations with varying soluble aggregate content were successfully prepared as shown in Table 11. A 16% sample with a remarkably low content of 1.9% soluble aggregates was included.

[0569] As shown in Figure 4, acidification of samples in a rheometer (all diluted to 4% protein before analysis) results in a significant increase in storage modulus (gel strength) in samples containing a large amount of soluble aggregates (for example, in sample A, a maximum of 1257 was observed at approximately 18 minutes (pH was 4.4)). On the other hand, a decrease in maximum gel strength is observed as the fraction of soluble whey protein aggregates decreases. For example, during acidification of a 16% sample (D) containing 1.9% acid-gellable protein, a maximum storage modulus of 7.1 Pa was measured. Such whey protein nanogel preparations are particularly useful in acidified / fermented products where a low degree of protein gelation is desirable, such as acidic whey protein beverages and high-protein yogurt. [Table 11]

[0570] Conclusion: Whey protein nanogel preparations produced under conditions favorable for the formation of low-volume soluble aggregates at high protein concentrations are particularly useful for low-viscosity acidified products because their viscosity remains low even after acidification.

[0571] Example 7: Use of a mixture between WPI and BLG for whey protein nanogel preparation We produced whey protein nanogel preparations by mixing a BLG composition with WPI, and demonstrated that mineral contributions from the WPI source inhibit the formation of whey protein nanogel preparations at high protein concentrations, ≥20-25 mM Na+K, and / or excessively high Ca:BLG ratios.

[0572] method: A 12% whey protein composition (A) was prepared by dispersing BLG isolate powder (see Example 1) in Milli-Q water and dissolving it by adjusting the pH to 6.0 using 3M NaOH. A 12% whey protein composition (B) was prepared by further titration to pH 6.4 using 3M NaOH.

[0573] The third whey protein composition (C) was thawed (frozen), diluted to 12% in MilliQ water, and adjusted to pH 6.0 using 3M NaOH. The protein composition of composition C is shown in Table 12.

[0574] 12% whey protein solutions, consisting of 100% 12% BLG A and 12% BLG A solution and 12% WPI solution in 80:20, 75:25, 66.7:33.3, and 50:50 ratios, were prepared by mixing appropriate volumes of BLG A and WPI.

[0575] Furthermore, a 66.7:33.3 mixture of BLG B and WPI was prepared to obtain a whey protein composition with a pH of 6.2.

[0576] All samples were heated at 95°C for 14 minutes and immediately cooled after heating. The state of the samples was evaluated by inverting the glass tubes. The distribution between soluble aggregates and nanogels was evaluated using Brix levels measured before and after centrifugation at 50.000xg for 1 hour. [Table 12]

[0577] Mineral content was determined using Analysis 14. The distribution between whey protein nanogels and soluble whey protein aggregates was determined by Analysis 3.

[0578] result: Table 13 shows whey protein nanogel preparations prepared by mixing BLG with WPI. All nanogel preparations had low total Na+K content, and the preparations remained liquid after heating at pH 6.0 when the calcium content was 0.0032 g / g BLG, while higher calcium content led to the formation of extensive gel clumps or gelation of the entire sample. Surprisingly, it was found that increasing the pH to 6.2 reduced gelation, and even with a calcium content of 0.0037 g / g BLG, it was possible to form a 12% whey protein nanogel preparation even with the presence of more ALA and CMP in the sample. [Table 13]

[0579] The non-denatured proteins found in the whey protein nanogel preparation were mainly composed of CMP.

[0580] Conclusion: Whey protein nanogel preparations can be manufactured when the protein concentration is high, in the presence of other proteins besides BLG, the calcium level is increased, the Na and K content is sufficiently low, and the pH is increased to compensate for the higher calcium level.

[0581] Example 8: Use of nanogels for the preparation of acidic beverages with low astringency The inventors observed that whey protein in nanogel form offers less astringency than other types of denatured whey. Astringency is not a taste but a sensation in the mouth, such as contraction of the cheek muscles and increased saliva production. Astringency can arise from the consumption of foods, such as unripe fruit, red wine, and heat-sterilized acidic protein beverages. In this example, the inventors investigated the low astringency of whey protein nanogels.

[0582] method The BLG nanogel preparation was prepared using the following modifications, as described in Example 2 "OPQ": In Example 1, 10% BLG characterized by the properties shown in Table 1 was adjusted to a Ca:BLG ratio of 0.0021 w:w using a 5% Ca(OH)2 slurry, and then further adjusted to 6.0 using 10% NaOH. Heat treatment was performed at 93°C for 10 minutes using a pilot-scale scraping heat exchanger, followed by cooling to 10°C. Finally, the nanogel preparation was concentrated to 20.4% protein on an MMS SW40 RO pilot unit using a spiral reverse osmosis membrane (Alfa Laval RO98pHt-65-263364) at a pressure of 20 bar, and spray-dried on an Anhydro MicraSpray MS 750 to produce nanogel powder.

[0583] 7.3 kg of whey protein nanogel powder having the properties described in Table 14 below was dispersed in 30.8 kg of desalted water in a Scanima mixer to produce an 18% BLG nanogel preparation, which was hydrated overnight at 10°C with gentle stirring. The dispersion was homogenized at 200 bar, then the pH was adjusted using 9% HCl, and diluted with desalted water to produce a 10% BLG nanogel solution with a pH of 3.5.

[0584] The nanogel solution was sterilized using an OMVE HT320 pilot plant UHT system configured to provide heat treatment at 120°C for 20 seconds using a plate heat exchanger, and then placed in 100 mL screw-cap bottles.

[0585] 1.1 kg of acidic BLG powder having the properties described in Table 14, prepared according to Example 2 of PCT application WO2020 / 002426, was dissolved in 8.9 kg of demineralized water to produce a 10% feed solution. The pH was adjusted to 3.51 and used without further adjustment. The BLG solution was sterilized using an OMVE HT320 pilot plant UHT system configured to provide heat treatment at 120°C for 20 seconds using a plate heat exchanger, and placed in 100 mL screw-cap bottles.

[0586] The viscosity of the beverage preparation was measured as described in Analysis 4. As outlined in PCT application WO2020 / 002435, the perceived level of astringency was evaluated using a modification in this example in which the undiluted sample was evaluated.

[0587] As described in PCT application WO2020 / 002435, astringency was evaluated on a scale of 0-15, where 0 is no intensity and 15 is high intensity. Brightness and turbidity were determined according to Examples 1.9 and 1.7 of PCT application WO2020 / 002435. Mineral, total solids, ash, and protein content of the raw materials, nanogel, and beverage composition were determined according to analyses 14, 12, 11, and 7 of this analysis, respectively.

[0588] result A 10% nanogel preparation characterized by a z-mean hydrodynamic diameter of 458 nm (Analysis 2), viscosity of 5.3 cP (Analysis 4), 89% nanogel, and 11% soluble aggregates was prepared, concentrated, and dried to produce nanogel powder. The nanogel powder was rehydrated and homogenized to facilitate its use in beverage compositions.

[0589] As shown in Table 15 below, a 10% whey protein nanogel beverage composition was prepared by heat treatment at 120°C / 20 seconds at pH 3.5 and compared with a 10% acidic BLG composition heat-treated at 120°C / 20 seconds. The resulting UHT-treated 10% reference beverage had a protein fraction consisting essentially of soluble aggregates and monomeric proteins (98%) and a small amount of nanogel (2%). [Table 14]

[0590] The nanogel beverage composition has high turbidity and lightness (L * This produced a beverage with a milky appearance as indicated by ), whereas, in contrast, the acidic BLG reference beverage was clear, as indicated by the amount of soluble aggregates and monomeric proteins (see Table 15).

[0591] The phosphorus content in nanogel beverages is below the detection limit, making such nanogel preparations particularly useful for patients with chronic kidney disease.

[0592] Sensory evaluation confirmed the inventors' initial findings, clearly demonstrating that the nanogel beverage composition had significantly reduced astringency compared to the clear reference beverage (see Table 15). This effect is thought to be closely related to the lower content of soluble aggregates and monomeric proteins in the milky white nanogel beverage compared to the clear BLG reference beverage, indicating that whey protein nanogels are particularly useful in UHT-treated acidic whey protein beverages. [Table 15]

[0593] conclusion A “milky white” nanogel beverage with high nutritional composition, turbidity, and whiteness was prepared. The beverage contained very low phosphorus levels, which is particularly important for the production of high-protein beverages for chronic kidney disease, but not limited to, those with intolerance to high levels of phosphorus. Sensory testing revealed that astringency was essentially absent in the UHT-treated nanogel beverage composition and was much lower than that of the UHT-treated BLG reference beverage.

[0594] Example 9: Use of nanogels for the preparation of acidic high-energy beverages The feasibility of using nanogels for the preparation of UHT-treated high-energy nutritional compositions under acidic conditions was evaluated.

[0595] method 10.8 kg of nanogel powder, prepared as described in Example 8, was dispersed in 68.5 kg of tap water at 65°C. The emulsifier, oil, and dry material components were mixed into a liquid for 15 minutes using a Brine Mixer Rotostat.

[0596] The pH was adjusted to 3.5 using 10% phosphoric acid, and the nutritional composition was homogenized at 150 bar. After homogenization, the nutritional composition was heat-treated on a tubular heat exchanger at 120°C for 30 seconds, cooled to 10°C, and then bottled in 100 mL sterile bottles.

[0597] Viscosity was measured according to Analysis 4, and astringency and acidity were determined as described in PCT application WO2020 / 002435, but without dilution before sensory testing.

[0598] result The inventors found that an acidic, high-energy beverage could be prepared, characterized by a remarkably low viscosity of 11.3 cP. In contrast, replacing the protein in nanogel form with an equal amount of protein derived from an acidic, unfractionated whey protein isolate was found to lead to clogging and blocking of UHT equipment. A low-viscosity, acidic, high-energy nutritional composition containing 10% protein, 4% fat, and 16% carbohydrates was prepared, providing a high energy density of 140 kcal / 100 mL in a small package.

[0599] Tasting of the nanogel composition revealed a surprisingly low level of astringency, scoring only 1 on a 0-15 (low-high) scale, compared to a score of 5 from the evaluation of the 10% BLG reference beverage in Example 8. Furthermore, the pH 3.5 nanogel beverage composition surprisingly had a sourness of only 2 on a 0-15 scale, despite its high protein concentration (10%) and no sample dilution (see, for example, Figure 15 of PCT application WO2020 / 002435).

[0600] conclusion A UHT-treated, low-viscosity, high-energy nutrient nanogel preparation with excellent sensory properties (low perceived astringency and sourness / acidity) was successfully prepared by combining the nanogel with fat and carbohydrate sources under acidic conditions. Attempts to generate a corresponding, yet unfractionated, natural whey protein isolate as a reference product resulted in a blocked UHT apparatus due to poorly controlled aggregation upon heating.

[0601] Example 10: Use of nanogels for the preparation of high-energy pH neutral beverages The feasibility of using nanogels for the preparation of UHT-treated high-energy liquid nutritional compositions under neutral pH conditions was evaluated.

[0602] method Whey protein nanogel powder was prepared as described in Example 8, and an 18% whey protein nanogel solution was prepared using this, which was hydrated overnight at 4°C and then homogenized at 200 bar. The homogenate was adjusted to pH 7.0 using 3M NaOH and preheated to 50°C in a water bath. To prepare the nutrient nanogel compositions shown in Table 16, 0.5 g / L of Grindsted Citrem LR10, rapeseed oil, sucrose, and the remaining water were mixed to prepare a sample of the homogenate. The weight fraction relative to the final liquid nutrient composition is provided. Finally, the nutrient composition was homogenized at 150 bar.

[0603] One mL of each nutritional composition was transferred to an HPLC vial, crimp-sealed, and heated by incubating the vial in an aluminum block at 150°C for 10 minutes. The heated samples were analyzed for their ability to flow upon inversion, and after removing the caps from the vials, the viscosity was measured according to Analysis 4.

[0604] result Nutritional nanogel compositions containing a carbohydrate source (range 8-17 w:w% sucrose), fat (rapeseed oil; range 4-9 w:w%), and nanogel (range 10-15 w:w%) were prepared. Surprisingly, all of the evaluated nanogel compositions remained liquid and flowed freely even after prolonged and extensive heating at 150°C for 10 minutes, regardless of the evaluated protein, fat, and carbohydrate content.

[0605] The viscosity remained remarkably low even at the highest protein dosage of 15% evaluated, and indeed, the nanogel enabled the preparation of a sterile nutritional composition with at least 200 kcal / 100 mL of energy by combining 15% protein, 8% fat, and 17% carbohydrates, as evidenced by the liquid state after heating at 150°C for 10 minutes and the measured low viscosity. [Table 16]

[0606] conclusion A low-viscosity, fluid, high-energy nutritional nanogel composition that resists heat treatment at a temperature of at least 150°C for at least 10 minutes can be prepared by heat treatment using an energy amount of at least 200 kcal / 100 mL. Therefore, high-protein beverages based on this whey protein nanogel can be made sufficiently thermally stable to withstand retort-type heat treatment, even at high protein concentrations.

[0607] Example 11: Use of acidic and pH-neutral whey protein nanogel powders and high-protein beverages Whey protein nanogel powders with acidic pH (pH 3.5) and neutral pH (pH 7.0) were prepared and used to prepare high-protein beverages.

[0608] method The nanogel powder was produced essentially as described in Example 8, using the following modifications: The nanogel preparation was concentrated to 16% protein and divided into three aliquots. Two of these were adjusted to pH 3.5 and 7.0 using 4.5% HCl and 2% NaOH, respectively. The three feeds were individually spray-dried to produce nanogel powder.

[0609] 20% nanogel dispersions of each nanogel powder (pH 3.5, 6.6, and 7.0) were rehydrated in desalted water and homogenized at 150 bar. The homogenates were diluted to 10-20% in desalted water, and the pH was readjusted as needed. 1 mL of the sample was transferred to an HPLC injection vial (Mikrolab, catalog number ML33003V) and crimped sealed. The sample was inserted into a 170°C aluminum block using a hole drilled to precisely fit the dimensions of the vial, ensuring efficient heat transfer. The sample was maintained at 170°C for 120 seconds, or at 90°C for up to 10 minutes, and then immediately cooled.

[0610] The initial indication of fluidity (liquid / gel) was determined by the ability to flow upon inversion of the vial, and viscosity was determined using Analysis 4. Particle size after heating was determined using a Malvern Mastersizer 3000 equipped with a HydroLV liquid dispersion unit. The heated nanogel solution was dropped into a water-containing dispersion unit under stirring at 1500 rpm until an obscuration of 8-10% was reached. Particle size was estimated using a RI of 1.4, an absorption coefficient of 0.01, and a refractive index of 1.33 for the solvent (water), assuming spherical particles when calculating particle size in Mastersizer 3000 software version 3.62.

[0611] result Nanogel preparations characterized by a particle size of 0.424 microns were successfully prepared, followed by pH adjustment, concentration, and drying to produce nanogel powders (total powder %w / w) with the following compositions: [Table 17]

[0612] Using nanogel preparations, we evaluated the available protein range for heat-treated, low-viscosity, still protein-rich nanogel beverages: [Table 18]

[0613] conclusion We successfully prepared powders with pH values ​​of 3.5, 6.6, and 7.0 and used them to produce both acidic and pH-neutral high-protein beverages.

[0614] A high-protein nutritional beverage was prepared by heat treatment of the following nanogel-containing beverage: • Heat to at least 18% pH 7.0 at 170°C for at least 120 seconds. • Heating to at least 20%, pH 7.0, at 90°C for at least 10 minutes. • Heating to at least 20%, pH 6.6, at 90°C for at least 10 minutes. • Heat to at least 14% pH 3.5 at 170°C for 120 seconds.

Claims

1. A method for producing a whey protein nanogel composition, a) To provide a whey protein solution having the following: -4-28% w / w of natural β-lactoglobulin (BLG) content, - A natural BLG content of at least 50% w / w relative to total protein, pH in the range of -5.8 to 7.5 - The weight ratio between total calcium and natural BLG as follows - At most 0.0041 ＊ pH -0.0209, and - At least 0.0037 ＊ pH -0.0234, but greater than 0, and - Total concentration of the following monovalent metal cations: - If the natural BLG content of the whey protein solution is less than 10% w / w, then at most 25 mM, - If the natural BLG content of the whey protein solution is at least 10% w / w, then at most 20 mM, b) Heat the whey protein solution to a temperature of at least 68°C for a period of time sufficient to form a suspension of whey protein nanogels having a z-average diameter of 150-1000 nm. c) Optionally, concentrate the suspension of whey protein nanogel to obtain a concentrated suspension of whey protein nanogel. d) Optionally, dry the dryer feed containing the whey protein nanogel derived from step b) or c). The method, including the method described above.

2. The method according to claim 1, wherein the whey protein solution contains 8-24% w / w of natural BLG.

3. The method according to claim 1 or 2, wherein the whey protein solution contains 12-28% w / w of natural BLG.

4. The method according to any one of claims 1 to 3, wherein the whey protein solution contains natural BLG in an amount of at least 60% w / w relative to the total protein.

5. The method according to any one of claims 1 to 4, wherein the whey protein solution contains natural BLG in an amount of at least 90% w / w relative to the total protein.

6. The method according to any one of claims 1 to 5, wherein the whey protein solution has a protein denaturation degree of at most 10% w / w relative to the total protein.

7. The method according to any one of claims 1 to 6, wherein the whey protein solution has a pH in the range of 5.8 to 6.

5.

8. The method according to any one of claims 1 to 7, wherein the whey protein solution has a total concentration of monovalent metal cations of at most 15 mM.

9. The method according to any one of claims 1-8, wherein the heating in step b) is carried out for a period of time sufficient to denature at least 95% w / w of the natural BLG.

10. The method according to any one of claims 1 to 9, comprising step c), wherein the concentrated suspension of whey protein nanogel contains a total amount of 21–35% w / w of protein.

11. The method according to claim 10, wherein the concentrated suspension of whey protein nanogel contains at most 6% of soluble whey protein aggregates.

12. The method according to any one of claims 1 to 11, comprising step d), wherein the dryer feed comprises a total amount of 21-35% w / w of protein.

13. The method according to any one of claims 1 to 12, wherein the whey protein nanogel composition is in the form of a powder, and the method comprises step d) drying a dryer feed comprising the whey protein nanogel derived from step b) or c).

14. - Whey protein nanogel in an amount of at least 90% w / w relative to total protein, - A maximum of 10% soluble whey protein aggregates, - Total BLG in an amount of at least 90% w / w relative to total protein, - Total amount of protein of at least 30% of the total solid A whey protein nanogel composition in powder form, comprising: The particles of the hydrated whey protein nanogel composition have a z-average diameter measured by dynamic light scattering in the range of 150-1000 nm, and the whey protein nanogel composition can be obtained by one or more methods according to claims 1-13.

15. A whey protein nanogel that can be obtained by one or more methods according to claims 1-13, wherein the whey protein nanogel is present in desalted water at a concentration of 20.0% w / w, and is subjected to 20°C and 300 s. －１ A whey protein nanogel that provides a viscosity of at most 50 cP at a shear rate.

16. 3. The use of a whey protein nanogel in a hydrated form having a z-average diameter of 150-1000 nm, and / or a whey protein nanogel composition in a hydrated form, as a protein source for reducing the astringency and / or acidity of a heat-treated protein beverage having a pH of 3.0-5.0, wherein the particles of the whey protein nanogel composition in a hydrated form have a z-average diameter measured by dynamic light scattering of 150-1000 nm. The whey protein nanogel and / or whey protein nanogel composition is - Can be obtained by one or more methods of claims 1-13, or - The whey protein nanogel composition according to claim 14, or - Use of the whey protein nanogel according to claim 15.

17. The use according to claim 16, wherein the whey protein nanogel provides at least 50% w / w of the total protein of the heat-treated beverage.

18. The use according to claim 16 or 17, wherein the heat-treated beverage contains a total protein amount of 2-35% w / w.

19. The use according to any one of claims 16-18, wherein the whey protein nanogel contains a total amount of at least 60% w / w of BLG.

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