Co-processed fibers and hydrocolliods, compositions, methods of making the same and food products obtained therefrom

Abstract

The invention provides a composition comprising a co-processed hydrocolloid and a plant based fiber, the process for preparation of the composition and it's use in food applications.

Description

[0001] IFF10037-WO-PCT2

[0002] 1

[0003] CO-PROCESSED FIBERS AND HYDROCOLLIODS, COMPOSITIONS, METHODS OF MAKING THE SAME AND FOOD PRODUCTS OBTAINED THEREFROM

[0004] FIELD OF THE INVENTION

[0005] The present invention is directed to new product compositions comprising 50-95% cellulose containing fibers and 5-50% anionic hydrocolloids, methods of making them and food products, comprising them.

[0006] BACKGROUND OF THE INVENTION

[0007] Microcrystalline cellulose, also known and referred herein as MCC, is widely used to enhance product properties within the food and pharmaceutical industry. For these purposes, MCC is preferably modified through a process known as "attrition," where hydrolyzed cellulose wet cake undergoes high shear mixing. During attrition, microcrystalline crystallites are broken down into fine particles, typically falling within the colloidal range. However, due to the uncharged nature of MCC, the crystalline particles tend to agglomerate or aggregate into larger structures upon drying— a phenomenon known as hornification. To address this issue, a protective hydrocolloid is introduced either before or during attrition but prior to drying. Negatively charged polymers serve as suitable protective hydrocolloids, with carboxymethyl cellulose (CMC) being the preferred choice due to its structural compatibility with MCC. These hydrocolloids effectively screen out the hydrogen bonds or other attractive forces between smaller particles, resulting in a readily dispersible powder. The protective hydrocolloid facilitates the re-dispersion of microcrystalline cellulose in water, resulting in a material commonly referred to as colloidal microcrystalline cellulose, colloidal MCC, or attrited microcrystalline cellulose.

[0008] Colloidal MCC, especially when modified with CMC, forms stable suspensions with little or no settling of the dispersed solids. US 3539365 (Durand et al), WO2018031859 Al (Tan et al) and WO2022125895A1 (Anankanbil et al) describes such colloidal MCCs.

[0009] Colloidal MCC serves as a crucial stabilizer for suspensions, including those containing solid particles in low-viscosity liquids, such as chocolate milk. In various food applications - ranging from canned foods, shell-stable spreads, and salads to frozen desserts, aerosol toppings, meat, dairy, and bakery products - colloidal MCC functions as a fat replacement or bulking agent, providing non-caloric filling and texture IFF10037-WO-PCT2

[0010] 2 modification. Colloidal MCC products are for example available under the brand names Avicel® and Gelstar®.

[0011] Because of the nature of its production, CMC is not considered "clean label" component, although still considered safe by regulatory authorities. This has prompted efforts to substitute CMC with a more "clean label" recognized hydrocolloid. In the literature it has, however, been reported difficult to co-process these negatively charged hydrocolloids (like alginates, pectin, carrageenan, xanthan gum, welan gum or gellan gum) with MCC because the material is too 'slippery' for effective attrition, which compromises the functionality of the MCC stabilizer. To tackle this, the use of an "anti-slip agent", such as a salt, acid or starch, has been utilized (e.g. patents W02019050598 (Yang et al.) and W02013085809 (Tan et al.), US 7462232 (Tuason et al.), 20050233046 Al (Krawczyk et al.)). The use of salts or acids as attrition aids, however, may have deleterious effects on production plants due to corrosive tendencies.

[0012] The production of colloidal microcrystalline cellulose (MCC), with a typical composition of 12-20% carboxymethyl cellulose (CMC) and 88-80% MCC, involves a series of carefully controlled steps. Initially, the MCC wet cake is subjected to an attrition process, such as extrusion. This process substantially subdivides the aggregated cellulose crystallites into more finely divided crystallite particles. As described above, to prevent the agglomeration or aggregation of these particles upon drying, CMC is added as a protective hydrocolloid. This hydrocolloid may be added at any stage before, during, or after attrition, but crucially before drying. The final step in the manufacturing process is the drying of the MCC-hydrocolloid wet cake. In commercial manufacturing, this is commonly achieved through spray-drying, as described in G. Thorens et al, Int. J. Pharm. (2015), 490, 47-54. By varying and controlling the conditions of the spray drying process, it is possible to manipulate the degree of agglomeration and moisture content, thereby obtaining the desired commercial grades of colloidal MCC. However, spray-drying presents its own challenges. It can only be performed on slurries with a high water content, necessitating the dilution of the MCC wet cake with water prior to spray-drying. A typical aqueous slurry for spray drying consists of approximately 10-20% colloidal MCC and 80-90% water. This high water content results in significant energy expenses due to the large amount of water that must be evaporated. Additionally, spray-drying equipment is costly, adding to the overall expense of the process. These challenges have highlighted the need for more efficient, sustainably, and cost-effective methods for producing colloidal MCC and has recently been overcome by drying the non-diluted colloidal MCC wet cake by the utilisation of mill drying as described in WO2022152760A1 (Petermann et al.). In this case it was possible to obtain higher viscosity of the impact IFF10037-WO-PCT2

[0013] 3 mill dried colloidal MCC compared to the spray dried version when activated by high shear. In this work it was not mentioned if the mill dried ingredient can provide stabilisation and suspension in a food application.

[0014] The present inventors tried to identify alternative cellulose-containing fibres suitable as a replacement for MCC in typical colloidal MCC applications. The applicants have unexpectedly found that co-processing subsequently followed by dry milling of a mixture of citrus fiber and CMC produces a stabilizer composition that has unexpected, good stabilising and suspension properties at very low dose level and yields a beverage with low viscosity on par with commercial low viscosity colloidal MCC types. The dry mill technology permits drying of the undiluted wet cake at a dry matter content significantly higher than what is achievable with spray drying.

[0015] It has not previously been disclosed that MCC can be replaced with another fiber type, such as citrus fiber, and that this co-processed ingredient can be dosed at a very low dose level (0.06-0.08%). Due to the environmentally friendly drying procedure and very low dose level, such a stabilizer composition provides significant commercial and industrial advantages.

[0016] Subsequently, driven by market demand for clean label solutions, this research extended to explore anionic hydrocolloids with a perceived cleaner label status compared to CMC. Our findings most unexpectedly revealed that other anionic hydrocolloids, such as pectin, in combination with a cellulose containing fiber materials, such as citrus fiber, efficiently could undergo the attrition and drying process without the need for processing aids by a careful selection of process conditions for both the attrition and drying process.

[0017] This CMC- and MCC free ingredient is able to provide stabilisation and suspension power at dose levels on par with existing low dosis colloidal MCC products (0.25%), but yields higher viscosity in the beverage, thereby makes addition of eg. carrageenan redundant to increase viscosity.

[0018] BRIEF DESCRIPTION OF DRAWINGS

[0019] Figure 1 Strain sweep IFF10037-WO-PCT2

[0020] 4

[0021] Figure 2 Strain sweep

[0022] Figure 3 Strain sweep

[0023] SUMMARY OF THE INVENTION

[0024] The invention provides a method to dry a co-processed hydrocolloid / fiber wet cake at very high dry matter content, where the resulting product afterwards can be activated by standard food production process conditions such as homogenization or high shear mixing, and thereby obtain a food ingredient that yields high suspension power.

[0025] The present invention relates to a process for producing a stabilizer composition comprising of a cellulose containing fiber with a negatively charged hydrocolloid. The invention covers the compositions, methods of production and food products comprising these co-processed ingredients.

[0026] The present inventors have surprisingly found it possible to provide a stabilizer composition made with replacement of MCC for another cellulose containing fiber and additionally to replace CMC with another charged hydrocolloid without significant loss of functionality, e.g. reduction of sedimentation in a beverage, compared to a stabilizer comprising MCC co-processed with CMC. This has been obtained by providing a composition that can be effectively co-processed by combining different cellulose containing fibers with different types of negatively charged hydrocolloids. By selecting the optimal process conditions, it is possible to transfer sufficient mechanical force to the cellulose fiber material and anionic hydrocolloid during the attrition process without the need to use "anti-slip agents" such as salts or acids.

[0027] The resulting wet cake can be dried by the utilization of an impact mill by judicious choice of process conditions to prevents hornification and retain the functionality obtained by the mechanical activation. The use of a dry mill to dry the wet cake permits the drying of the wet cake at a dry matter content significantly higher than what is achievable with spray drying. This results in a product that is not only highly functional but also produced through a method that is more efficient, sustainable, and cost-effective than spray drying.

[0028] The resulting co-processed composition can easily be dispersed in consumable products such as food, beverage, and many other products, including, cool / ambient milk products, e.g., chocolate milk or creamers, without the use of sequestrants. IFF10037-WO-PCT2

[0029] 5

[0030] In another aspect, the present invention relates to a process for producing a mechanically activated and dry milled cellulose containing fiber and anionic hydrocolloid mixture to produce a stabilizer composition of any one of the aspects above, comprising the steps of

[0031] (a) A product blend composition consisting of 55-95% cellulose containing fiber and 45-5% anionic hydrocolloid is mixed.

[0032] (b) Applying a high-shear attrition process to the moist mixture of fiber, hydrocolloid, and water in the absence of an attrition aid to form an extrudate, and

[0033] (c) Optionally adjusting the amount of water added to the fiber / hydrocolloid wet cake such that the mixture before drying has a dry matter between 30% and 50%.

[0034] (d) Dry milling of the fiber / hydrocolloid / water mixture in a single device capable of milling and drying in combination to achieve a co-processed cellulose containing fiber / anionic hydrocolloid blend.

[0035] Additionally, the invention provides consumable products, such as foods and beverages, comprising the stabilizer composition of the invention. Ideally such consumable products will attain suspension stability (as defined herein).

[0036] DETAILED DESCRIPTION OF THE INVENTION

[0037] Unless otherwise specified all references cited herein are incorporated by reference in their entirety. The present invention will use the following definitions:

[0038] The term "invention" or "present invention" as used herein is a non-limiting term and is not intended to refer to any single embodiment of the particular invention but encompasses all possible embodiments as described in the specification and the claims.

[0039] The terms "co-processing" and "co-processed" are used interchangeably to mean a process that effectively reduces the particle size and increases molecular interactions between fibers and hydrocolloids. The term "co-processing " refers to application of high shear forces to a mixture of a cellulose containing fiber and at least one polysaccharide. Suitable processing conditions may be obtained, for example, by co-extruding or kneading. Co-processing is also referred to in the literature as "co-attrition". IFF10037-WO-PCT2

[0040] 6

[0041] "Colloid" and "Colloidal" as used herein refers to particles that may be suspended in a mixture and are used interchangeably in this invention. Colloidal particles may be of any suitable size if they can form colloidal suspensions. Average particle sizes in the order of about 0.1 to 10 microns are typical for colloidal particles.

[0042] The term suspension stability, as used herein, means that when the co-processed fiber / hydrocol- loid particles are dispersed in a liquid, e.g., aqueous medium, milk, etc., containing insoluble components, e.g., cocoa, calcium, etc., those particles are effectively suspended forming a stabilized suspension having a homogenous appearance without significant separating, aggregating, or settling of the insoluble particles.

[0043] The term "consumable product" means a food or beverage product that is formulated for human or animal consumption.

[0044] The term "hydrocolloid" means a carbohydrate containing more than three monosaccharide units per molecule, the units being attached to each other in the manner of acetals, and therefore capable of hydrolysis by acids or enzymes to monosaccharides. Preferred hydrocolloids of the invention are those that contain acidic sugar residues such as for example, galacturonic acid, glucuronic acid, mannuronic acid and / or guluronic acid residues. It is particularly preferred where those residues reside on a main polymer chain in the polysaccharide. Hydrocolloids useful in the present invention include (but is not limited to) carrageenans (iota, lambda, kappa, kappa-2, mu, nu, theta, or mixtures thereof), alginate, pectins (including high ester, low ester pectins, and acetylated pectins (such as beet pectin)), xanthan gums, agar gums, wellan gums, gellan gums, carboxymethyl cellulose and mixtures thereof. Semi-refined carrageenans are also useful in the present invention (these are less purified forms of the carrageenans that may contain some of the structural components of the seaweed such as cellulose). In one specific embodiment of the invention CMC is used as hydrocolloid, in another embodiment of the invention a low ester pectin is used.

[0045] Carboxymethyl cellulose, herein referred to as CMC, are preferably alkali metal carboxymethyl cellulose. Examples are the sodium, potassium or ammonium salts of CMC. Sodium salts of CMC are the most preferred. CMC is characterized by, among other things, the degree of substitution (DS). The term "DS" refers to the degree of carboxymethyl substitution per anhydro glucose unit and means the average number of hydroxyl groups substituted with carboxymethyl groups per anhydro glucose unit. The DS is IFF10037-WO-PCT2

[0046] 7 measured according to ASTM D 1439-03 "Standard Test Methods for Sodium Carboxymethylcellulose; Degree of Etherification, Test Method B: Nonaqueous Titration". The theoretical maximum of DS in CMC is 3.0 since each anhydro glucose unit contains three hydroxyl groups. CMC is also characterized, by the viscosity. A "low viscosity" CMC has a viscosity from 25 cP to 3300 cP as measured in a 2% solution and a "high viscosity" CMC has a viscosity of 500cP -9200 cP in a 1 % solution, both measured in water at 25°C using a Brookfield viscometer at 60 rpm and a Spindle No. 1. Preferred herein is a CMC with DS in the range 0.65-0.9 and viscosity 300-600 cP in a 2% solution.

[0047] The term pectin covers a range of polysaccharides having the common feature that they are rich in galacturonic acid. The "degree of esterification" (DE) means the extent to which free carboxylic acid groups contained in the galacturonic acid units of pectin have been methyl esterified. The resultant pectin is referred to as "high ester pectin" ("HE pectin" for short) if more than 50% of the carboxyl groups are esterified. The resultant pectin is referred to as a "low ester pectin" ("LE pectin" for short) if less than 50% of the carboxyl groups are esterified. The structure of pectin, in particular the degree of esterification, determines its physical and / or chemical properties. For example, pectin gelation depends on the chemical nature of pectin, especially the degree of esterification and degree of polymerization. Preferred pectin types for use herein comprises low ester pectin types, for example, but not limited to, pectin types with %DE between 25-35 and molecular weight between 25.000 and 35.000 Da.

[0048] Alginate, a family of linear binary co-polymers, consists of (l->4)-linked 0-D-mannuronic acid (M) and a-L-guluronic acid (G) residues. These co-polymers exhibit widely varying composition and sequence. Investigating the sequential structure of alginates reveals several fractions with distinct compositions. Notably, there are homopolymeric molecules containing guluronic and mannuronic acid, as well as nearly equal proportions of both monomers, resulting in numerous MG or GM dimer residues. Alginate is a true block copolymer, featuring homopolymeric regions of M and G, referred to as M-blocks and G-blocks, respectively. These blocks are interspersed with alternating structures, forming MG- or GM-blocks. Alginate with a high proportion of continuous G-blocks exhibits enhanced gelling potential in the presence of multivalent ions, such as calcium ions found in milk systems. Conversely, an alginate rich in continuous M- blocks yields a lower gelling potential. Alginates suitable for use herein can comprise significant portions of continuous M- block polymers or can comprise significant portions of alternating block (MG or GM) IFF10037-WO-PCT2

[0049] 8 regions. It can be preferred to exclude alginates having significant portions of continuous G-block polymers.

[0050] A cellulose-containing fiber material refers to fibers primarily composed of cellulose— a natural polymer found in plant cell walls. These fibers can be obtained from various plant-based sources, including, but not limited to: wood pulp, cotton, hemp, bamboo, and from cell wall materials of an edible fruit or vegetable such as citrus, apple, banana, pineapple, mango, carrot, soy, sugar-beet, potato ect. In two specific embodiments of the invention citrus fiber is used. The citrus fiber can originate from citrus peel from a wide variety of citrus fruit, non-limiting examples of which include oranges, tangerines, limes, lemons, and grapefruit. In one preferred embodiment, the citrus fiber contains high ester pectin. In another preferred embodiment the citrus fiber does not contain pectin.

[0051] Processing Methods

[0052] In a preferred embodiment the co-processed stabilizer composition comprises Citrus fiber and CMC in a weight ratio between 70:30 and 90:10, preferably between 80:20.

[0053] In another preferred embodiment the co-processed stabilizer composition comprises Citrus fiber and pectin in a weight ratio between 50:50 and 70:30, preferably between 60:40.

[0054] Co-processing:

[0055] The cellulose containing fiber and hydrocolloid are co-processed, in the absence of process aiding compounds to form the co-processed composition. Processing methods are common and well known in the art (see for example US20130090391 Al (Tan et al.) and US Patent US9828493 B2 (Tan et al.).

[0056] Useful compounders are, for example, granulators, kneaders, extruders, presses, or roller mills, wherein the dry mixture and liquid is homogenized by applying shear forces and compounding, such as a twin- screw compounder. Co-rotating as well as counter-rotating machines are suitable. So-called divided trough kneaders with two horizontally arranged agitator blades that engage deeply with one another and that perform a mutual stripping action, as in the case of twin-screw compounders are particularly suitable. Suitable single-shaft, continuous kneaders include the so-called Reflector® compounders, which are high performance mixers of modular construction, consisting of a multi-part, heatable and coolable mixing cylinder and a unilaterally mounted blade mixer (manufacturer: Lipp, Germany). Also suitable are so- IFF10037-WO-PCT2

[0057] 9 called pinned cylinder extruders or Stiftconvert® extruders (manufacturer: Berstorff, Germany). The pins incorporated in the housing serve as abutments to prevent the kneaded material rotating together with the shaft. Kneader mixers with so-called double-blade sigma stirrers (manufacturer: Fima, Germany) in a horizontal assembly are particularly suitable. The blades operate at different speeds and their direction of rotation can be reversed. A stirred vessel with a vertically arranged mixer shaft is also suitable if suitable flow baffles are mounted on the vessel wall in order to prevent the kneaded mass rotating together with the stirrer shaft, and in this way an intensive mixing action is imparted to the kneaded material (manufacturer: Bayer AG). Also suitable are double-walled mixing vessels with a planetary stirrer and inline homogenizer.

[0058] Mill drying:

[0059] The thus obtained moist mixture of fiber and hydrocolloid is subsequently subjected to mill drying in a mill drying device according to the process of the present invention to produce the mill dried co-processed stabilizer. Before drying, an additional amount of water may be blended with the extrudate to avoid the individual particles to agglomerate or hornify upon the drying process.

[0060] The present invention involves a process where the mill-drying of co-processed fiber and hydrocolloid is performed in a singular apparatus capable of both milling and drying concurrently. This apparatus is referred to as a "mill-drying device". In these mill-drying devices, the operations of milling and drying are integrated, with a preference for at least partial simultaneity. These devices are functionally and structurally distinct from devices solely used for drying materials. For instance, drying devices primarily utilize thermal energy. However, mill-drying devices significantly employ both mechanical and thermal energy. The term "mechanical energy" is defined here as the energy, usually electrical, necessary to initiate and maintain the operation of the mill-drying device, such as rotational motion. The term "thermal energy" refers to the energy supplied by the pre-heated drying gas that is introduced into the mill-drying device.

[0061] A mill-drying device, beneficial in the process of the current invention, typically includes a mill-drying chamber. This chamber is fitted with one or more inlets for the wet cake and gas, and with one or more grinding inserts such as grinding pins, rods, bars, plates, or disks. These grinding inserts are generally in motion, preferably rotating, when the mill-drying chamber is operational, and they achieve milling of the wet cake through impact and / or shearing. Drying is typically achieved through a combination of hot gas and mechanical energy. Hot air is most commonly used, but hot nitrogen gas can also be utilized. The hot IFF10037-WO-PCT2

[0062] 10 gas and the wet cake can be introduced into the mill-drying chamber via separate inlets, typically with hot gas from the bottom and moist colloidal wet cake at a side entrance via a feed screw system connected to the mill-drying chamber. Alternatively, the moist colloidal wet cake can be introduced into the gas stream and subsequently into the mill-drying chamber via the gas stream. Depending on the position of the inserts in the mill-drying chamber, the moist colloidal wet cake can first be partially dried before it is milled, or the moist colloidal wet cake can first be partially milled before it is dried, or milling and drying can be conducted simultaneously. However, it is crucial that milling and drying are conducted in a single device where milling and drying are done in combination.

[0063] Mill-drying of the wet cake can be conducted in a known mill-drying device, for example in an impact mill, preferably a gas-swept impact mill, more preferably an air-swept impact mill, wherein the wet cake is subjected to an impacting and / or shearing stress as well as to drying.

[0064] Particle size, particle morphology, bulk density and flowability of the mill dried wet cake can be controlled and / or adjusted by the design and / or operation of the mill-drying device, such as the type and number of grinding inserts like grinding pins, rods, bars, plates or disks or the circumferential speed of the mill-drying chamber. The larger the number of grinding inserts is in a given mill-drying chamber and / or the higher the circumferential speed of a given mill-drying chamber is, the smaller are generally the median particle sizes of the mill dried product. Preferred designs and operations of the mill-drying device are described in more detail below and in the examples.

[0065] Preferred air-swept impact mills are Ultra Rotor mills (Altenburger Maschinen Jaeckering, Germany), Contra-Selector PPS (PALLMANN Maschinenfabrik GmbH & Co. KG, Germany), or Turbofiner PLM mills (PALL- MANN Maschinenfabrik GmbH & Co. KG, Germany). Gas classifier mills are also useful air-swept (gas- swept) impact mills, for example, the Hosokawa Alpine Air Classifier mill - ZPS Circoplex Hosokawa Micron Ltd., Cheshire, England. Other preferred mill-drying devices are flash mill dryers; they are commercially available, for example from Hosokawa under the trademark Drymeister (DMR). Other suitable mills and mill-type dryers are, for example hammer mills, screen-type mills, pin mills, or centrifugal impact mills, disk mills, or preferably classifier mills. IFF10037-WO-PCT2

[0066] 11

[0067] Air or nitrogen gas can be used for drying. In the process of the present invention the gas fed into the milldrying device, more specifically the mill-drying chamber of the mill-drying device, typically has a temperature of 200°C or less. A gas stream having the above-mentioned temperature can be created in various ways. For example, a gas stream can be separated from the ground and dried product, and the resulting solid-free gas stream, or a portion thereof, can be cooled in a cooling system, e.g., using water as coolant. This resulting cooled gas stream can be fed into the mill-drying device. Alternatively, the entire amount of cooled gas can be re-heated, e.g. in a natural gas burner. To bring the re-heated gas to the desired temperature for feeding into the mill-drying device, a separate stream of cold gas can be combined with the hot gas stream before feeding the gas stream into the mill-drying device.

[0068] The gas and the wet cake are generally fed via separate inlets into the mill-drying chamber, typically gas from the bottom and wet cake at a side entrance via a feed screw system connected to the mill-drying chamber resulting in an upward flow of product and gas, while the wet cake is being contacted with one or more grinding inserts, such as grinding pins, rods, bars, plates or disks inside the mill-drying chamber. Alternatively, the wet cake can be fed into the gas stream and subsequently via the gas stream into the mill-drying chamber.

[0069] Dry particles formed from the impact mill drying can be reconstituted in a desired aqueous medium or solution to form the compositions, edible food products, and industrial applications described herein.

[0070] Spray drying technique:

[0071] Spray drying is a process of forming a dry powder from a liquid or slurry by rapid drying with hot air. All spray dryers use a kind of atomizer device to disperse the slurry into a controlled fine drop-size spray cloud. The feed slurry is pumped to the atomizer. The dried product is separated / discharged out from the hot humid exhaust air in a cyclone and or a bag filter housing. The necessary drying air flow is driven by a fan.

[0072] Prior to spray drying, the feed can be exposed to various down-stream processing such as wet milling, homogenization, shear pump treatment, pH adjustment and pasteurization etc.

[0073] Commercially available spray dryers may be a single stage, two stage, Multi Stage Dryer or a mix of these. There exist many different variations of layout and design of spray dryers with either counter or counter current air flow. The spray dryer can be equipped with an internal fluid bed and or an external fluid bed. IFF10037-WO-PCT2

[0074] 12

[0075] The internal bed can both dry and create powder agglomeration. The external fluid bed can further dry and cool the product before the packaging. Fines from the cyclone and the external fluid bed (if available) can be led back to the atomization cloud. The atomizer device can either be an atomizer wheel, a rotary disk, pressure nozzle(s) or two fluid atomization. Pressure and two fluid nozzles drying can either be top spray or fountain upwards spray. High pressure nozzle drying requires a high-pressure pump to generate the desired pressure to the nozzle. The pressure nozzle design and the actual orifice pressure have a huge impact of the spray pattern inside the chamber.

[0076] Before entering the drying chamber, the air is heated to a desired temperature. After heating, the air is led to an effective air distributor commonly on top of the drying chamber, which distributes the air in the correct pattern in the drying chamber. The air throughput rate generally depends on various factors and the desired characteristics of the final dried product.

[0077] The feed suspension is pumped to the atomizer devise by various pump types or using a high-pressure pump. In embodiments of the invention, the feed temperature is 1 - 98 °C.

[0078] The air outlet temperature can automatically be controlled by the pump speed flow. In embodiments of the invention the air inlet temperature is 120 - 300 °C. The desired powder moisture content in the powder is closely linked to the air outlet temperature. A high air outlet temperature decreases the water content in the powder. In embodiments of the invention, the air outlet temperature is 60 -120 °C, depending on the spray dryer design / layout.

[0079] The product is discharged from the wet humid air by a cyclone and or a bag filter housing.

[0080] Hot gas, which is used to dry the liquid, is typically sucked through the drying chamber by means of a fan. For example, when atomization is achieved with an atomizer wheel, a greater air throughput typically increases the moisture content and bulk density of the final powder product, reduces the retention time in the dryer, reduces the heat load expose of the spray-dried particles, reduces the off-colouring of the product and reduces production costs associated with the spray-drying.

[0081] For two fluid nozzle and pressure atomization the air throughput in combination with the nozzle design, the air or product pressure determine and affect the particle size distribution, bulk density, and moisture content. IFF10037-WO-PCT2

[0082] 13

[0083] The spray dryer uses an atomization device means (i.e., a mechanism that breaks up the liquid into droplets). The liquid pass through the atomization, as it enters the drying chamber. The centrifugal force of an atomizer wheel or rotary spinning disk at high RPM speed throws out the liquid in a spray, as it enters the wheel or disk. High pressure nozzle(s) creates a spray by forcing the liquid through an orifice at high pressure. A two fluid nozzle creates a spray by contacting the liquid with a compressed gas. In some embodiments, the spray dryer comprises an atomizer wheel. The desired rotational speed of the atomizer wheel generally depends on various other process parameters and the desired characteristics of the final dried product. For example, variation of the atomizer speed can typically be used to control the moisture content, the bulk density, and particle size distribution in the final dried product. In general, slower atomizer speeds result in a product with a greater moisture content, greater bulk density, and greater particle size distribution compared to a product produced using a faster Atomizer speed. A faster atomizer speed typically creates finer droplets in the atomization cloud. Normally, the finer droplets dry faster than larger droplets, and the resulting product has a smaller particle size distribution relative to a product produced with slower atomizer speed. The smaller particles can be more difficult to separate / discharge in the cyclone and or bag filter housing, ultimately translating into less product percent yield recovery. Particles made with a faster atomizer speed will generally have more entrapped and void air both inside the particles and between the particles. A faster atomizer speed can often be used to allow for an increased feed rate and / or air throughput to the dryer while still producing a product with low moisture content. Faster atomizer speed can be particularly useful with feeds having a high viscosity, high solids content / % Brix value. Lower atomizer speeds can be particularly useful with feed solutions having a low solids content or Brix value. Slower atomizer speeds can often be used to achieve good instant properties of the dried product, such as wettability, solubility and dispersibility. For high pressure atomization, pressure typically can be varied to control the moisture content, the bulk density and the particle size distribution in the final dried product. In general, increasing the pressure results in effects similar to those resulting from increasing atomizer wheel speed. For two fluid nozzle atomization, nozzle size typically can be varied to control the moisture content, the bulk density and the particle size distribution in the final dried product. In general, the two fluid nozzle inner diameter, the air cap setting, the air throughput, the compressed air pressure all effect the physical powder properties, the moisture content, the product flowability, the bulk density etc. In embodiments of the invention the atomizer wheel atomization has tip periphery speed 60 - 160 m / sec. In embodiments of the invention the high-pressure nozzle atomization is set at a pressure IFF10037-WO-PCT2

[0084] 14 from 50 - 600 bar. In embodiments of the invention single stage, two stage or MSD spray dryers and or a combination of other various dryer design is used.

[0085] Oven drying:

[0086] A lab drying oven is a specialized device used in laboratories for removing moisture from samples, maintaining temperature uniformity, and ensuring sample integrity.

[0087] Applications

[0088] The stabilizer composition of this invention aligns with consumer preference for natural ingredients and can be employed in a wide array of food products, including but not limited to emulsions, beverages, sauces, soups, syrups, dressings, films, dairy and non-dairy milks and creamers, frozen desserts, cultured foods, bakery fillings, and bakery cream. It can be used to deliver flavoring and coloring agents.

[0089] The food products may comprise various edible materials and additives, such as proteins, fruit or vegetable juices, pulps, and fruit-flavored substances. They can also include other edible ingredients like mineral salts, protein sources, acidulants, sweeteners, buffering agents, pH modifiers, stabilizing salts, and more. Additional components like flavorings, colorings, preservatives, pH buffers, nutritional supplements, process aids, etc., can be added as per requirement. These ingredients can be soluble or insoluble, with the latter being suspended in the food product.

[0090] The food products can range from dry mix products (e.g., instant sauces, gravies, soups, cocoa drinks) to low pH dairy systems (e.g., sour cream / yogurt, yogurt drinks, stabilized frozen yogurt), baked goods, and can also serve as a bulking agent in non-aqueous and low moisture food systems.

[0091] Proteins suitable for these food products include food proteins and amino acids beneficial to various species. These proteins can be derived from animal or plant sources, including milk and milk products, egg and egg-derived proteins, nut proteins, sorghum, legume proteins such as soy and soy products, and rice proteins. They can be used in any form, including liquid, condensed, or powdered. For powdered proteins, pre-hydration may be desirable for added stability of the resulting beverage. The quantity of protein added will depend on the desired outcome, especially when used in conjunction with a fruit or vegetable juice. IFF10037-WO-PCT2

[0092] 15

[0093] It should also be noted that the food / beverage compositions may be processed by heat treatment in any number of ways. These methods may include, but are not limited to, Low Temperature Long Time (LTLT), High Temperature Short Time (HTST), Ultra-High Temperature (UHT) and Extended Shelf Life (ESL) processes. These beverage compositions may also be retort processed, either by rotary retort or static retort processing. Some compositions, such as juice-added or natural or artificially flavored soft drinks may also be cold processed. Many of these processes may also incorporate homogenization or other high shear / high compression methods. There may also be co-dried compositions, which can be prepared in dry-mix form, and then conveniently reconstituted for consumption as needed. The resulting beverage compositions may be refrigerated and stored for a commercially acceptable period of time. In the alternative, the resulting beverages may be stored at room temperature, provided they are filled under aseptic conditions.

[0094] The described compositions can act as stabilizers suitable for use in the beverage industry. The compositions, after drying to powder form, can be mixed with an aqueous solution to form a colloidal mixture that, in some embodiments, can maintain its colloidal properties for a long period of time. Some of the edible food products are beverages, protein and nutritional beverages, mineral fortified beverages, dairybased beverages, and non-dairy based beverages including, but not limited to, those that are heat treated, for example, by pasteurization, ultra-pasteurization, or retort processes.

[0095] The typical concentrations of the stabilizer of the present invention used in the above products can range from 0.05% to about 3.5% by wt. of total products, and in some instances 0.2 to 2.0% by wt. of total products. In particular the compositions of the invention are well suited for stabilization of beverages, particularly dairy milk beverages or plant protein beverages. For these applications, the present stabilizer compositions may be present in an amount of 0.06-0.30% by weight of the beverage.

[0096] EXAMPLES

[0097] General methods:

[0098] Starting materials for producing the microcrystalline fiber / hydrocolloid composition IFF10037-WQ-PCT2

[0099] 16

[0100] The CMC used is commercially available from IFF® under the trademark Texturecel 1000 PA07, with a DS in the range 0.65-0.9 and viscosity 300-600 cP in a 2% solution.

[0101] The pectin used is extracted from lime or lemon peel and enzymatically de-esterified. The %DE is 27.2 and MW is 32000 Da.

[0102] The citrus fibers used as cellulose containing fiber material were commercially available from Ingredion under the trademark "FIBERTEX™ CF 502 citrus fiber" and from Herbafood Ingredients GmbH under the name "Herbacel® AQ® Plus Citrus".

[0103] FIBERTEX™ CF 502 citrus fiber has a water holding capacity of 13.0, cellulose content of 66%, no pectin content was detected. Viscosity measured at shear rate 0.0199 1 / s: 63.0, shear rate 0.91 1 / s: 1.17, shear rate 9.54 1 / s: 0.222.

[0104] Herbacel® AQ® Plus Citrus fiber has a water holding capacity of 7.6, cellulose content of 69%, pectin content of 17% with %DE 60.8. Viscosity measured at shear rate 0.0199 1 / s: 591, shear rate 0.91 1 / s: 8.56, shear rate 9.54 1 / s: 0.856.

[0105] Determination of degree of substitution for CMC

[0106] The DS is measured according to ASTM D 1439-03 "Standard Test Methods for Sodium carboxymethylcellulose; Degree of -o-etherification, Test method B; Non-aqueous Titration", which is performed as follows: The treatment of a solid sample of the CMC with glacial acetic acid at boiling temperature releases an acetate ion quantity equivalent to the sodium carboxymethyl groups. These acetate ions can be titrated as a strong base in anhydrous acetic acid using a perchloric acid standard solution. The titration end point is determined potentiometrically. Other alkaline salts of carboxylic acids (e. g. sodium glycolate and disodium diglycolate) behave similarly and are co-titrated.

[0107] Determination of viscosity for CMC

[0108] The viscosity of CMC is measured as a 2% by weight solution in water at 20 °C and at a shear rate of 2.55 s 1 using a Haake VT550 Viscotester according to the following method: A 2% by weight solution was prepared: 196.0 g deionized water (water in CMC is subtracted) was placed in 250 ml screw cap bottle. 4 g (dry weight) of the CMC was added onto the surface. After closing the bottle, it was vigorously shaken and placed on a rolling device until a clear solution was obtained (48 h). Afterwards the solution was allowed to settle without stirring / rolling over night. The viscosity was analyzed using a Haake VT550 IFF10037-WO-PCT2

[0109] 17

[0110] Viscotester at 20°C (+ / - 0.1 °C) and at a shear rate of 2.55 s"l. The MV DIN sensor and the MV cup was used. The solution of the CMC was filled in the cup until the ring was reached. The solution was pretempered at a 20°C water bath. After the system was closed the solution was tempered for 3 min without shearing, then the analysis was started. After shearing for 110 s at 2.55 s'l 15 data points were taken and averaged in 20 s.

[0111] Determination of degree of esterification for pectin and citrus fiber

[0112] Determination of degree of esterification (DE) and galacturonic acid content (GA). The degree of esterification was determined as described below.

[0113] Weigh 5 g of the pectin sample or citrus fiber to the nearest 0.1 mg into a 250 ml beaker and add a mixture of 100 ml 60% aqueous 2-propanol and 5 ml cone hydrochloric acid. Stir on a magnetic stirrer for 10 minutes. Filter through a dried and pre-weighed 30 ml coarse glass filter funnel with reduced vacuum. Wash with six 15 ml portions of HCI-60% 2-propanol mixture. Then wash with 60% aqueous 2-propanol (6-8 portions of 20 ml) until the filtrate is free from chloride (test with a solution of 1.7 g silver nitrate in 100 ml of distilled water). Finally wash with approx. 30 ml of 100% 2-propanol. Dry for 2% hours in an oven at 105°C. Cool in a desiccator. Weigh (acidic alcohol insoluble solids, AAIS).

[0114] Pipette 20.00 ml of 0.5 N sodium hydroxide using 20 ml volumetric pipette into a beaker and mix with 20.00 ml of 0.5 N hydrochloric acid, which has been transferred using a 20 ml volumetric pipette. Add two drops of a solution of phenolphthalein (1 g of phenolphthalein is dissolved in 100 ml of 96% ethanol) indicator and titrate with 0.1 N sodium hydroxide. Record the volume V0.

[0115] Weigh exactly one tenth of the washed and dried pectin into a 250 ml Erlenmeyer flask and moisten with 2 ml 96% ethanol. Place the flask on a magnetic stirrer and slowly add 100 ml of boiled and cooled deionised water. Avoid splashing. Stir until all the pectin is completely dissolved. Add five drops of the solution of phenolphthalein and titrate with 0.1 N sodium hydroxide. The volume is recorded as VI in ml. Add 20.00 ml of 0.5 N sodium hydroxide and shake vigorously. Allow the content to rest for 15 minutes in order to saponify the ester groups. Add 20.00 ml 0.5 N hydrochloric acid and shake until the pink color disappears. Add three drops of the solution of phenolphthalein and titrate with 0.1 N sodium hydroxide until achieving a faint persisting pink color, recording the volume of 0.1 N sodium hydroxide required as V2 ml. IFF10037-WO-PCT2

[0116] 18 100

[0117] %GA = 19.41 * (Vi + V2- VQ) weight [g]

[0118] Determination of Molecular weight for pectin

[0119] The relative average molar mass of pectin is calculated from the specific viscosity of a diluted pectin solution where aggregation of pectin molecules is suppressed, so that each pectin molecule can be fully hydrated. 0.09% pectin is dissolved in a 1% Sodium Metaphosphate solution at pH 4.5 and viscosity measured on a falling ball viscometer (Lovis 2000 ME microviscometer from Anton Paar) with water bath at 21°C. The relation between intrinsic viscosity and molar mass is [q]=K*Ma, where K is a constant and a is a form factor, which is one for strict linear molecules and 0 for globular molecules. For simplicity a linear form factor is chosen, and the constant K is set to 6.25*10-6. With these approximations the result is expressed as a relative average molar mass.

[0120] Water holding capacity for cellulose containing fibers

[0121] Procedure for determination of water holding capacity for fibers.

[0122] 1. Record the weight of a centrifuge tube - without lid (50 mL) = A

[0123] 2. Add 10 mL demineralized water to the tube.

[0124] 3. Add sample (as is) = B

[0125] 4. Add demineralized water up to the 45mL graduation in the 50mL centrifuge tube

[0126] 5. Stir for 30 min at room temperature

[0127] 6. Centrifuge the sample for 20 minutes at 4696 G - adapt deaccelerate speed if the residue is not compacted enough at the end

[0128] 7. Discard the supernatant and let the tube stand up-side down for ~ 5 minutes

[0129] 8. Weight the tube = C

[0130] Water holding capacity = (C-(A+B)) / B

[0131] Determination of pectin% and cellulose%

[0132] The sugar free dried sample is methanolysed and the released sugar units are determined by GC / FID after silylation. IFF10037-WO-PCT2

[0133] 19

[0134] Cellulose is calculated based on amount of quantified glucose using cellulose as a standard material. Pectin is quantified from galacturonic acid using pectin as a standard material. Apparatus used is Agilent 7890A serial CN10903121 equipped with Flame Ionization Detector. A Restek column RTX-5 cat. No. 10224 is used for separation.

[0135] Viscosity profile for cellulose containing fiber material

[0136] A 0.6% slurry (based on dry matter) is made from the fiber in 60 °C demineralized water. The fiber is hydrated for 10 min under stirring at 1000 rpm, before the resulting slurry is 2-stage homogenized twice at 150 bar first stage and 50 bar second stage. The gel is stored in a fridge (4 °C) overnight before the viscosity profile is determined. Shear rate viscosity was determined using a stress-controlled MCR 502 rheometer equipped with a Double Gap geometry (DG26.7). Temperature is controlled by C-PTD200 temperature controller. The specific protocols implemented in a series of experiments at 20°C are low sweeps were conducted at shear rates from 0.02-100 1 / s recording 100 points in a logarithmic ramp over 300s.

[0137] Mechanical activation / Co-processing

[0138] A dry solid blend of the cellulose containing fiber and the hydrocolloid are mixed at a defined ratio of 55- 95% cellulose containing fibers and 5-45% anionic hydrocolloid.

[0139] The process can be described in two steps: (1) The hydration and mechanical co-processing of the dry solid blend in a Werner & Pfleiderer twin-screw kneader (also referred to as compounder) and (2) the dry milling of the compounder outlet material (also referred to as dough) in the ALTENBURGER Ultrarotor II impact mill. Between the two steps is a dough disintegrating device (paddle mixer, manufactured by ALTENBURGER) that reduces the size of the kneader outlet material to improve the mill feed consistency.

[0140] Step 1: Hydration / co-processing in kneader

[0141] The fiber material was mixed with the hydrocolloid in a plough shear mixer in a defined ratio. This mixture (containing a moisture content of 9%) is fed manually into the hopper of the Gericke loss-in-weight- feeder. The dry blend was fed continuously at a feed rate of 20 kg / h into a commercially available continuous twin-screw 5” compounder (Werner & Pfleiderer twin-screw kneader) with heating and cooling jacket. In the compounder water of a temperature of 5° C was continuously added before the first kneading zone resulting in a moisture level of about 45-65%. The water flow is adjusted to achieve the defined kneader outlet material moisture level. The compounder jacket was supplied with tab water of approximately 12° C. The twin-screws of the kneader can be operated with different rotational speed to 92 rpm. IFF10037-WO-PCT2

[0142] 20

[0143] In all experiments the rotational speed was set to 70% of the maximum rotational speed. A screw design with three kneading zones was applied. After the wet product was processed through the compounder one time, the resulting wet cake optionally was passed through the compounder two more times with the addition of more water to decrease the dry matter content before the dry milling step.

[0144] The processing conditions are listed in Table 1.

[0145] Dry milling

[0146] The resulting wet cake was fed into an air swept impact mill (Ultrarotor II "S" impact mill, Altenburger Maschinen Jaeckering GmbH, Hamm, Germany) via a mill feed unit (Altenburger Maschinen Jaeckering GmbH, Hamm, Germany). The bottom blades of the vessel agitator pressed the filter cake into a single augur screw mounted at the bottom of the vessel. The wet product was forced through a perforated plate (d=14 mm of voids) directly into the side of the impact mill between the first and second grinding stage. The mill was equipped with seven grinding stages. The bottom three grinding stages were equipped with standard grinding bars. Turbo-bars were installed in the top four grinding stages. A co-rotating finger sifter wheel with twelve blades was installed on the top of the 7th grinding stage. The interior of mill jacket had the standard Altenburger corrugated stationary grinding plates.

[0147] The rotor of the impact mill was operated at a circumferential speed up to 114 m / s (or 4444 rpm=100%). A hot gas stream was fed with 1200 m3 / h into the bottom air inlet of the mill. Air or nitrogen gas can be used for drying. In the process of the present invention the gas fed into the mill-drying device, more specifically the mill-drying chamber of the mill-drying device, typically has a temperature of 200°C or less, preferably 160 °C or less, and in some embodiments of 130 °C or less, such as 120 °C or less, or even 110°C or less. Typically, the gas fed into the mill-drying device has a temperature of 50 °C or more, preferably of 60 °C or more, more preferably of 65 °C or more. The mill outlet temperature was controlled to be 90 °C + / -5 °C. This allowed achieving a final product moisture level of below 6%. A cyclone was used to separate the dried product from the nitrogen. The dried samples were directly collected after the milling-drying step by sieving through an Allgaier tumbler screening machine (Allgaier, Uhingen, Germany) equipped with a 500 micron screen to remove oversize. The processing conditions are listed in Table 1.

[0148] Table 1. The processing conditions for co-processing and dry milling. IFF10037-WO-PCT2

[0149] 21

[0150] Experimental sample 1 was passed through the compounderthree times with constant dry matter content of 38% (62% moist). Sample 4 was passed through the compounder one time with dry matter content of 47% (moist 53%). Sample7 were passed through the compounder one time with dry matter of 54% (moist 46%), and subsequently the wet cake was passed through the compounder two times more, where an additionally amount of water with a temperature of 5°C were added to reach a dry matter content of the wet cake of 39% (61% moist) for the last pass. All three samples were milled with a gas flow through the mill of 1200 m3 / h.

[0151] Spray drying.

[0152] The wet cakes resulting from the co-processing step were dissolved in water, adjusting the dry matter content to achieve a viscosity suitable for efficient spray drying. To obtain a homogenous slurry, the mixture was treated with a Silverson Stator rotor Mixer®. The liquid suspension was sieved to remove any fine lumps before the spray drying.

[0153] A GEA Niro / LP Kolding Production Minor co-current spray dryer with extended chamber height spray dryer equipped with an atomizer wheel was used to spray dry the Feed slurry. The conditions for the spray drying step are shown in Table 2 and the specific dry matter and moisture content for spray drying is seen in Table 3.

[0154] Table 2. Conditions used for spray drying. IFF10037-WO-PCT2

[0155] 22

[0156] Table 3. Specific conditions for co-processing and spray drying of experimental samples 2, 5 and 8.

[0157] Oven drying The wet cake was disintegrated and spread out in a thin layer on a tray, before it was heated in the oven at 90°C for 24 h. After oven drying the samples were milled at 2000 pm at a Retsch Ultra Centrifugal Mill ZM 200, and afterwards sieved at 212pm.

[0158] Dynamic rheological measurements of Sample Dispersions For dynamic rheological measurements, a sample dispersion was prepared using demineralized water that had a solids content of 2.6 wt.%, based on the total weight of the dispersion. The dynamic moduli (elas- tic / storage modulus, G' and loss / viscous modulus, G") were determined using a stress-controlled MCR IFF10037-WO-PCT2

[0159] 23

[0160] 502 rheometer equipped with a Double Gap geometry (DG26.7). Temperature is controlled by C-PTD200 temperature controller.

[0161] The specific protocols implemented in a series of experiments at 20 °C are a strain sweep, and a flow sweep separated by 5 minutes of wait time to allow sample recovery. Samples were always pre-sheared prior to these measurement steps using a shear rate of 50 1 / s for 120 sec, and a wait time of 300s. Strain sweep test were performed at an angular frequency of 0.5 Hz and 1-1000% strain amplitude. Flow sweeps were conducted at shear rates from 0.02-100 1 / s recording 100 points in a logarithmic ramp over 300s.

[0162] Apparatus

[0163] Homogenisator

[0164] Samples has been produced at two different homogenizers, i) Lab scale homogenizer, ii) pilot scale homogenizer. i) A lab scale homogenizer, Brand: Gea Niro Soavi; Type: Panda Plus 200, was used for preparing samples for viscosity profile of fiber-material. ii) A pilot scale homogenizer, Brand: Gea Niro Soavi; Type: NS2006L, was used for producing chocolate milk samples for chocolate milk for benchtop stability evaluation. ill) A BOS homogenizer, Model MG2-350B, capacity 200L / h was used for preparation of UHT plant based beverages and UHT flavored milk.

[0165] Comparative example A

[0166] The commercial Avicel® BV1416 sold by IFF.

[0167] Comparative sample B

[0168] A dry blend consisting of 80% of the commercially available citrus fiber Herbacel® AQ® Plus Citrus from Herbafood Ingredients GmbH and 20% of the CMC type "Texturecel 1000 PA07", with a DS in the range 0.65-0.9 and viscosity 300-600 cP in a 2% solution.

[0169] Comparative sample C

[0170] A dry blend consisting of 60% of the commercially available citrus fiber FIBERTEX™ CF 502 citrus fiber from Ingredion and 40% pectin with %DE 27.2 and MW 32000 Da. IFF10037-WO-PCT2

[0171] 24

[0172] Comparative sample D

[0173] The commercial Avicel® RC591 sold by IFF.

[0174] Example 1

[0175] The commercially available citrus fiber Herbacel® AQ® Plus Citrus from Herbafood Ingredients GmbH was mixed with CMC type "Texturecel 1000 PA07". The ratio between citrus fiber and CMC was 80:20 based on dry matter. This blend was loaded into the compounder and passed through three times with constant dry matter content of 38% (62% moist). The resulting wet cake was subsequently dried using the dry milling technology. Process conditions are showed in Table 1.

[0176] Example 2

[0177] The same wet cake as produced in Example 1 was dried using spray drying. The conditions are shown in Table 3.

[0178] Example 3

[0179] The same wet cake as produced in example 1 was dried using oven drying and subsequently milled.

[0180] Example 4

[0181] The commercially available citrus fiber FIBERTEX™ CF 502 citrus fiber from Ingredion was mixed with a pectin with %DE 27.2 and MW 32000 Da. The ratio between citrus fiber and pectin was 60:40 based on dry matter. This blend was loaded into the compounder and passed through one round with dry matter content of 47% (moist 53%). The resulting wet cake were subsequently dried using the dry milling technology. Process conditions are showed in Table 1.

[0182] Example 5

[0183] The same wet cake as produced in example 5 was dried using spray drying. The conditions are shown in Table 3.

[0184] Example 6

[0185] The same wet cake as produced in example 5 was dried using oven drying. IFF10037-WO-PCT2

[0186] 25

[0187] Example 7

[0188] The commercially available citrus fiber FIBERTEX™ CF 502 citrus fiber from Ingredion was mixed with a pectin with %DE 27.2 and MW 32000 Da. The ratio between citrus fiber and pectin was 60:40 based on dry matter. This blend was loaded into the compounder were passed through first one time with a dry matter of 54% (moist 46%), this wet cake were then passed through the compounder two times more, where an additionally amount of water with a temperature of 5°C were added to reach a dry matter content of the wet cake of 39% (61% moist) for the last pass. The resulting wet cake were dried using the dry milling technology. Process conditions are showed in Table 1.

[0189] Example 8

[0190] The same wet cake as produced in example 9 was dried using spray drying. The conditions are shown in Table 3.

[0191] RHEOLOGY

[0192] Strain sweep - Example C, 4, 5 and 6

[0193] Based on rheology using a strain sweep methodology, Examples 4 and 5, produced by applying an impact mill and spray dryer, respectively, result in a significantly improved storage modulus (G') mean value in the linear viscoelastic region. This indicates a stronger network, which relates to a higher suspension power of this material compared to the oven-dried material (Example 6) and the comparative Example C. Thus, more functionality is obtained by applying these specific drying technologies. Results shown in Figure 1.

[0194] Strain sweep - Example C, 7 and 8

[0195] Based on rheology using a strain sweep methodology, Examples 7 and 8, both produced by applying additional shear through three passes on the Kneader followed by impact milling and spray drying, respectively, show that Example 7 results in a significantly improved storage modulus (G') mean value in the linear viscoelastic region. This indicates a stronger network, which relates to a higher suspension power of this material compared to the spray-dried material (Example 8) and the comparative Example C. Thus, more functionality is obtained by applying impact milling compared to spray drying. Results shown in Figure 2. IFF10037-WO-PCT2

[0196] 26

[0197] Strain sweep - Example B, 1, 2 and 3

[0198] Based on rheology using a strain sweep methodology, Examples 1 and 2, produced by applying an impact mill and spray dryer, respectively, result in a significantly improved storage modulus (G') mean value in the linear viscoelastic region. This indicates a stronger network, which relates to a higher suspension power of this material compared to the oven-dried material (Example 3) and the comparative Example B. Thus, more functionality is obtained by applying these specific drying technologies. Results shown in Figure 3.

[0199] Shear-rate viscosity profile

[0200] Shear-rate viscosity profiles were determined for Examples B, C, 1, 2, 3, 4, 5, 6, 7, and 8. The same trend observed using the strain sweep methodology was concluded. The trend of shear-rate viscosity was similar to the G' value when comparing the examples. Data is not included.

[0201] FOOD APPLICATIONS

[0202] HTST (High Temperature Short Time) flavored milk

[0203] Samples of HTST chocolate milk were prepared following the formulations shown in Table 4.

[0204] Table 4: Formulations for pasteurized chocolate milk tests

[0205] All powders were dry blended (sugar, cocoa powder, and co-processed ingredient) and mixed with low fat milk (fat content 1.5 %) to make up to 100%. HTST chocolate milk was prepared in 1.5 L batches. The HTST procedure was as described below: i. The pre-blended dry ingredients were added into the milk and mixed at medium shear with a IFF10037-WO-PCT2

[0206] 27 propeller mixer for 10 min; ii. The chocolate milk was pre-heated to 85°C for 15 sec; ill. Downstream homogenization was performed at a total pressure of 200 bar first stage and 50 bar second stage; iv. The chocolate milk was then cooled immediately to <20°C and filled in sterile plastic bottles Samples were evaluated after a period of two weeks of storage at refrigeration temperature (4°C).

[0207] The visual parameters described in Table 5 were assessed.

[0208] Table 5: Visual parameters for chocolate milk evaluation IFF10037-WO-PCT2

[0209] 28

[0210] Evaluation of chocolate milk was carried out according to Table 5. Results of pH, viscosity and visual observation after 1-week storage at 4°C are described in Table 6 (comparative examples) and Table 7 (experimental examples). pH was measured using a calibrated pH meter (Inolab). Viscosity was measured at 8-12 °C with a Brookfield LV viscometer with spindle #1 at 60 rpm for 30 sec.

[0211] Table 6: Week 1 evaluation results for comparative example A, B and C tested in HTST chocolate milk and stored under refrigerated conditions. IFF10037-WO-PCT2

[0212] 29

[0213] The chocolate milk comprising comparative sample A (commercial colloidal MCC product) dosed in 0.25% provided a beverage with good dispersion properties, low viscosity and with acceptable creaming level. For the comparative sample B, dosed in 0.08%, the ingredient did not provide suspension power or vis- cosity, but had slight tendency to gelation. The chocolate particles were sedimented to the bottom of the bottle already after 24 h storage. Chocolate milk comprising comparative sample C, dosed in 0.25%, showed unacceptable level of phase separation and an unacceptable level of gelation.

[0214] Table 7: Week 1 evaluation results for experimental example 1 to 8 tested in HTST chocolate milk and stored under refrigerated conditions. IFF10037-WO-PCT2

[0215] 30

[0216] The composition of the experimental sample 1 to 3 is a co-processed blend of Citrus fiber and CMC, which has been dried with three different methods. Chocolate milk beverages comprising 0.08% shows that the drying technique mill drying (example 1) yields a beverage with similar properties as the commercial comparative example A, but dosed less than 1 / 3 lower. Slight ripples were observed but considered acceptable. Example 2 (spray drying) did provide an ingredient with stabilisation and suspension power, but with twice as high viscosity as example 1 (dry milling). Example 3 (oven dried) did not provide suspension or stabilisation.

[0217] The composition of the experimental sample 4 to 8 is a co-processed blend of pectin and citrus fiber, which has been mechanical activated and dried with different methods. Experimental sample 4 to 6 originated from same wet cake, which has been run through the compounder one time, and then dried with three different drying techniques. Experimental sample 7 and 8 additionally originates from the same wet cake, which has been run through the compounder three times, and then dried with either mill drying or spray drying.

[0218] The results in Table 7 shows that a beverage stabilised with co-processed pectin and citrus fiber dosed in 0.25% yields a higher viscosity compared to comparative sample A. Both comparative sample 4, 5, 7 and 8 can provide suspension power and stability in the chocolate beverage with an acceptable evaluation after 1 week's storage at refrigerated conditions.

[0219] UHT (Ultra high temperature) flavored milk

[0220] Samples of UHT calcium fortified milk were prepared following the formulations shown in Table 8. Milk calcium 995 was supplied by Fonterra NZMP, which contained 29-30% calcium. Avicel® RC591 was used as comparative stabilizer.

[0221] Table 8: Formulations for UHT calcium fortified milk tests

[0222] Formulation Formulation 1 Formulation 2 Formulation 3

[0223] (% wt.) (% wt.) (% wt.)

[0224] Milk Calcium 995 0.15 % 0.15 % 0.15 %

[0225] Stabiliser Example 1 0.04 % 0.06 % IFF10037-WO-PCT2

[0226] Comparative sample D MCC RC591 0.15 %

[0227] Pasteurized milk Up to 100 % Up to 100 % Up to 100 %

[0228] All powders were dry blended (Milk calcium 995 powder, and co-processed ingredient or MCC RC591) and mixed with pasteurized milk (fat content 3.5 %) to make up to 100%. UHT calcium fortified milk was prepared in 10 L batches. The UHT procedure was as described below:

[0229] 1. The pre-blended dry ingredients were added into the preheated milk at 65°C and mixed at medium speed with a Silverson high shear mixer for 10 min.

[0230] 2. Subsequently, the calcium fortified milk was homogenized at 200 bar (1st stage) / 40 bar (2nd stage);

[0231] 3. The calcium fortified milk was then gone through a UHT thermaliser at 138 °C holding for 4 seconds.

[0232] 4. The UHT treated milk was immediately cooled to 20°C and filled in sterile PET bottles.

[0233] Samples were evaluated after a period of four weeks of storage at 20°C, 42°C and 55°C. The visual parameters described in Table 5 were assessed.

[0234] Result

[0235] During shelf life storage, calcium fortified milks with co-processed citrus fiber / CMC compound showed no sedimentation and phase separation across all temperature conditions (Table 9). The co-processed citrus fiber / CMC showed less sedimentation, less marbling and better flowability than colloidal MCC RC 591 at 55°C storage 4 weeks. This indicated the co-processed citrus fiber exhibited excellent network control under high temperature.

[0236] Table 9: Shelf life assessment of calcium fortified milk

[0237] 55°C 4 weeks storage assessment

[0238] Sample Sedimentation Creaming Marbling Flow property Phase separation

[0239] Formulation 1 0.0 4.0 1.0 1.0 0

[0240] Formulation 2 0.0 4.0 0.5 1.0 0

[0241] Formulation 3 1.0 4.0 2.0 2.0 0 IFF10037-WO-PCT2

[0242] 32

[0243] 42°C 4 weeks storage assessment

[0244] Sample Sedimentation Creaming Marbling Flow property Phase separation

[0245] Formulation 1 0.0 3.0 0.0 1.0 0

[0246] Formulation 2 0.0 3.0 0.0 1.0 0

[0247] Formulation 3 1.0 3.0 0.0 1.0 0

[0248] 20°C 4 weeks storage assessment

[0249] Sample Sedimentation Creaming Marbling Flow property Phase separation

[0250] Formulation 1 0.0 3.0 0.0 0.0 0

[0251] Formulation 2 0.0 3.0 0.0 1.0 0

[0252] Formulation 3 1.0 3.0 0.0 0.0 0

[0253] In summary, the Experimental sample 1 (co-processed citrus fiber / CMC) worked effectively in calcium fortified milk at all storage conditions. Typical dosage was 0.04%, which showed an advantage of dosage over colloidal MCC. UHT (Ultra high temperature) plant based beverages

[0254] Samples of UHT peanut milk were prepared following the formulations shown in Table 10. Skim milk powder and sodium caseinate were supplied by Fonterra NZMP, which contained 33 % and 90 % protein, respectively. Peanut paste was supplied by Yinlu Foods, which contained 40 % fat. Emulsifier mono-di glyceride Dimodan HP-C was provided by Danisco China. Xanthan gum XG80 was supplied by Danisco China. Comparative sample D RC591 was used as comparative stabilizer.

[0255] Table 10: Formulations for UHT peanut milk tests

[0256] Formulation Formulation 4 Formulation 5

[0257] (% wt.) (Comparative sample)

[0258] (% wt.)

[0259] Skim milk powder 0.8 % 0.8 %

[0260] Peanut paste 3.0 % 3.0 % IFF10037-WO-PCT2

[0261] 33

[0262] Sugar 7.0 % 7.0 %

[0263] Sodium caseinate 0.15 % 0.15 %

[0264] Emulsifier Mono-di glyceride 0.10 % 0.10 %

[0265] Trisodium citrate 0.04 % 0.04 %

[0266] Sodium bicarbonate 0.05 % 0.05 %

[0267] Sodium tripolyphaste 0.03 % 0.03 %

[0268] Stabiliser Example 1 0.04 %

[0269] Stabiliser MCC RC591 0.17 %

[0270] Stabiliser Xanthan gum 0.05 % 0.05 %

[0271] Demineralised water Up to 100 % Up to 100 %

[0272] All powders were dry blended and mixed with demineralised water to make up to 100%. UHT peanut milk was prepared in 10 L batches. The UHT procedure was as described below: i. The pre-blended dry ingredients were added into the preheated RO water at 75°C and mixed at medium speed with a Silverson high shear mixer for 10 min; ii. The peanut paste was then added and mixed at medium shear for 5 min; ill. Subsequently, the peanut milk was homogenized at 300 bar (1ststage) / 60 bar (2ndstage); iv. The peanut milk was gone through another homogenization at 250 bar (1ststage) / 50 bar (2ndstage) and then was UHT thermalized at 138 °C holding for 30 seconds. v. The UHT treated milk was immediately cooled to 20°C and filled in sterile PET bottles

[0273] Samples were evaluated after a period of four weeks of storage at 20°C, 42°C and 55°C. The visual parameters described in Table 5 were assessed. The product viscosity was determined by a Brookfield viscometer (US) with a S60 spindle at 30rpm.

[0274] Results Table 11 shows co-processed citrus fiber / CMC leads to comparable viscosity and pH with colloidal MCC RC591 in peanut milk.

[0275] Table 11: pH and viscosity of peanut milk

[0276] Sample pH Viscosity

[0277] S60 30rpm (cP) IFF10037-WO-PCT2

[0278] 34

[0279] Formulation 4 7.27 13.3

[0280] Formulation 5 7.22 8.0

[0281] During shelf life storage, peanut milk stabilized co-processed citrus fiber / CMC compound has shown slightly less creaming and marbling than colloidal MCC RC591 at 55°C 4 weeks storage (Table 12). At 42°C and 20°C storage, there was no difference in shelf life stability between co-processed citrus fiber / CMC compound and colloidal RC 591.

[0282] Table 12: Shelf life assessment of peanut milk

[0283] 55°C 4 weeks storage assessment

[0284] Sample Sedimentation Creaming Marbling Flow prop- Phase separa- erty tion

[0285] Formulation 4 0.0 3.0 0.0 1.0 0

[0286] Formulation 5 0.0 4.0 1.0 1.0 0

[0287] 42°C 4 weeks storage assessment

[0288] Sample Sedimentation Creaming Marbling Flow prop- Phase separa- erty tion

[0289] Formulation 4 0.0 3.0 0.0 0.0 0

[0290] Formulation 5 0.0 3.0 0.0 0.0 0

[0291] 20°C 4 weeks storage assessment

[0292] Sample Sedimentation Creaming Marbling Flow prop- Phase separa- erty tion

[0293] Formulation 4 0.0 2.0 0.0 0.0 0

[0294] Formulation 5 0.0 2.0 0.0 0.0 0

[0295] In summary, the co-processed citrus fiber / CMC (example 1) worked effectively in peanut milk at all storage conditions. Typical dosage was 0.04%, which showed an advantage of dosage over colloidal MCC.

[0296] The invention discloses the following clauses:

[0297] 1. A composition comprising a co-processed and dried blend of 50-95% cellulose-containing fiber material and 5-50% hydrocolloid based on dried weight, optionally containing up to 10% water.

[0298] 2. The composition of any of the preceding clauses, wherein the blend comprises 60-80% cellulose-con- taining fiber material and 20-40% hydrocolloid. IFF10037-WO-PCT2

[0299] 35

[0300] 3. The composition of any of the preceding clauses, wherein the blend comprises 80% cellulose-contain- ing fiber material and 20% hydrocolloid.

[0301] 4. The composition of any of the preceding clauses, wherein the blend comprises 60% cellulose-contain- ing fiber material and 40% hydrocolloid.

[0302] 5. The composition of any of the preceding clauses, wherein the cellulose-containing fiber material comprises a plant-based fiber with or without pectin.

[0303] 6. The composition of any of the preceding clauses, wherein the cellulose-containing fiber material comprises wood pulp, cotton, hemp, bamboo, and from cell wall materials of an edible fruit or vegetable such as citrus, apple, banana, pineapple, mango, carrot, soy, sugar-beet, potato.

[0304] 7. The composition of clause 6, wherein the cellulose-containing fiber material is a citrus fiber.

[0305] 8. The composition of clause 7, wherein the citrus fiber can originate from citrus peel from a wide variety of citrus fruits, such as oranges, tangerines, limes, lemons, and grapefruit.

[0306] 9. The composition of clauses 7-8, wherein the citrus fiber contains high ester pectin.

[0307] 10. The composition of clauses 7-8, wherein the citrus fiber does not contain pectin.

[0308] 11. The composition of any of the preceding clauses, wherein the hydrocolloid comprises carrageenans such as iota, lambda, kappa, kappa-2, mu, nu, theta, or mixtures thereof, alginate, pectins including high ester, low ester pectins, and acetylated pectins such as beet pectin, xanthan gums, agar gums, wellan gums, gellan gums, carboxymethyl cellulose and mixtures thereof.

[0309] 12. The composition of any of the preceding clauses, wherein the hydrocolloid is selected from carboxymethyl cellulose or pectins including high ester, low ester pectins, and acetylated pectins such as beet pectin, and mixtures thereof.

[0310] 13. The composition of any of the preceding clauses, wherein the composition is selected from pectins and citrus fiber or carboxymethyl cellulose and citrus fiber.

[0311] 14. The composition of any of the preceding clauses, wherein the composition is selected from CMC and citrus fiber at a level of 0.02% to about 3.5% by weight in the final drink.

[0312] 15. The composition of clause 14, wherein the composition is selected pectin and citrus fiber at a level of 0.2-2% by weight in the final drink. IFF10037-WO-PCT2

[0313] 36

[0314] 16. The composition of any of the preceding clauses, wherein the composition is selected from CMC and citrus fiber at a level of 0.06-0.30% by weight of the final drink.

[0315] 17. The composition of clauses 14-15, wherein the composition is selected from CMC and citrus fiber at a level of 0.08-0.25% by weight in the final drink.

[0316] 18. The composition of any of the preceding clauses, wherein the composition is spray dried or dry milled.

[0317] 19. The composition of any of the preceding clauses, wherein the composition is dry milled.

[0318] 20. The composition of any of the preceding clauses, wherein the composition has a water content of below 10%.

[0319] 21. The composition of clause 18, wherein the composition has a water content of below 5%.

[0320] 22. The composition of clause 19, wherein the composition has a water content of below 3%.

[0321] 23. The composition of any of the preceding clauses, wherein the composition comprising CMC and citrus fiber has a viscosity of above 20 cP as measured according to the examples, at a dosage of 0.08%

[0322] 24. The composition of any of the preceding clauses, wherein the composition comprising CMC and citrus fiber has a viscosity of above 25 cP as measured according to the examples, at a dosage of 0.08%

[0323] 25. The composition of any of the preceding clauses, wherein the composition comprising CMC and citrus fiber has a viscosity of below 75 cP as measured according to the examples, at a dosage of 0.08%

[0324] 26. The composition of any of the clauses 1-20, wherein the composition comprising pectin and citrus fiber has a viscosity of above 25 cP as measured according to the examples, at a dosage of 0.25%

[0325] 27. The composition of any of the clauses 1-20, wherein the composition comprising pectin and citrus fiber has a viscosity of above 35 cP as measured according to the examples, at a dosage of 0.25%

[0326] 28. The composition of any of the clauses 1-20, wherein the composition comprising pectin and citrus fiber has a viscosity of above 50 cP as measured according to the examples, at a dosage of 0.25%

[0327] 29. The composition of any of the clauses 1-20, wherein the composition comprising pectin and citrus fiber has a viscosity of above 75 cP as measured according to the examples, at a dosage of 0.25%

[0328] 30. The composition of any of the clauses 1-20, wherein the composition comprising pectin and citrus fiber has a viscosity of below 100 cP as measured according to the examples, at a dosage of 0.25% IFF10037-WO-PCT2

[0329] 37

[0330] 31. The composition of any of the preceding clauses, wherein the composition provides a stabilising effect as measured by phase separation at or below 1 after 1 week, as measured according to the examples.

[0331] 32. Use of a composition of any of the preceding clauses for application in food, and beverages.

[0332] 33. The use according to clause 30, wherein the composition is used at a concentration of 0.02%-0.5% by weight.

[0333] 34. The use according to clause 31, wherein the composition is used at a concentration of 0.05-0.3% by weight.

[0334] 35. A process for preparing the composition according to any of the clauses 1-29, comprising a. Mixing fiber and hydrocolloid b. Mechanical activation having a moisture content of 40-70%, followed by c. Dry grinding.

[0335] 36. The process of clause 33, comprising a. Mixing fiber and hydrocolloid as a dry blend, b. Mechanical activation having a moisture content of 40-70%, by addition of water in the coprocessing step, followed by, c. Dry grinding.

[0336] 37. The process of clauses 33-34, wherein the mechanical activation is performed 1-3 times.

[0337] 38. The process according to clause 33, wherein the co- processing is performed by adding water to the dry blend during the process, until a moisture level of about 45-65% is reached.

[0338] 39. The process of clause 35, wherein the dry grinding is performed on a dry mill.

[0339] 40. A composition comprising dried blend of 50-95% plant based fiber and 5-50% hydrocolloid based on dried weight according to any of the clauses 1-29, obtainable by the process of any of the clauses 33- 35.

Claims

IFF10037-WO-PCT238CLAIMS1. A composition comprising a co-processed and dried blend of 50-95% cellulose-containing fiber material and 5-50% hydrocolloid based on dried weight, optionally containing up to 10% water.

2. The composition of any of the preceding claims, wherein the cellulose-containing fiber material comprises wood pulp, cotton, hemp, bamboo, and from cell wall materials of an edible fruit or vegetable such as citrus, apple, banana, pineapple, mango, carrot, soy, sugar-beet, potato.

3. The composition of claim 2, wherein the vegetable fiber is a citrus fiber.

4. The composition of any of the preceding claims, wherein the hydrocolloid comprises carrageenans such as iota, lambda, kappa, kappa-2, mu, nu, theta, or mixtures thereof, alginate, pectins including high ester, low ester pectins, and acetylated pectins such as beet pectin, xanthan gums, agar gums, wellan gums, gellan gums, carboxymethyl cellulose and mixtures thereof.

5. The composition of claim 4, wherein the hydrocolloid is selected from carboxymethyl cellulose or pectins including high ester, low ester pectins, and acetylated pectins such as beet pectin, and mixtures thereof.

6. The composition of any of the preceding claims, wherein the composition is selected from pectins and citrus fiber or carboxymethyl cellulose and citrus fiber.

7. The composition of any of the preceding claims, wherein the composition is spray dried or dry milled.

8. The composition of any of the preceding claims, wherein the composition is dry milled.

9. The composition of any of the preceding claims, wherein the composition has a water content of below 10%.

10. The composition of any of the preceding claims, wherein the composition comprising CMC and citrus fiber has a viscosity of above 20 cP as measured according to the examples, at a dosage of 0.08%11. The composition of any of the claims 1-20, wherein the composition comprising pectin and citrus fiber has a viscosity of above 25 cP as measured according to the examples, at a dosage of 0.25%12. Use of a composition of any of the preceding claims for application in food, and beverages.

13. The use according to claim 12, wherein the composition is used at a concentration of 0.02%-0.5% by weight.IFF10037-WO-PCT23914. A process for preparing the composition according to any of the claims 1-11, comprising a. Mixing fiber and hydrocolloid b. Mechanical activation having a moisture content of 40-70%, followed by c. Dry grinding.

15. The process of claim 14, wherein the mechanical activation is performed 1-3 times.

16. A composition comprising dried blend of 50-95% plant based fiber and 5-50% hydrocolloid based on dried weight according to any of the claims 1-12, obtainable by the process of any of the claims 14-15

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