extruded granules

CN115996647BActive Publication Date: 2026-10-30FIRMENICH SA
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Patent Information

Application Number
CN202180052358.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Priority Date
2020-11-10
Filing Date
2021-11-08
Publication Date
2026-10-30
Estimated Expiration
2041-11-08

AI Technical Summary

Technical Problem

这种涂层通常是通过使用流化床或滚筒喷射熔融固体脂肪来实现的,因此需要额外的工艺步骤

Benefits of technology

[0164]在与这种产品有关的大量文献中可以找到其中可以掺入本发明颗粒的家居护理或织物护理基料。这些配方并不保证在这里的详细描述,其无论如何都是无法详尽无遗的。配制这样的消费品领域的技术人员完全能够根据他的一般知识和可用文献来选择合适的组分。

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Abstract

The present invention relates to the field of delivery systems. More specifically, the present invention relates to extruded particles, preferably flavor extruded particles, comprising a solid fat coating. The present invention also relates to a process for preparing said extruded particles.
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Description

Technical Field

[0001] This invention relates to the field of delivery systems. More specifically, this invention relates to extruded granules, preferably flavored extruded granules comprising a solid fatty coating (i.e., a hydrophobic coating). The invention also relates to methods for preparing said extruded granules and consumer products comprising said extruded granules. Background Technology

[0002] Consumer demand for delivery systems is becoming increasingly important and is driving the development of new delivery systems.

[0003] Granular delivery systems are commonly used in the flavoring or aromatization field because they are easy to measure, handle, and prepare.

[0004] Depending on the application, the delivery system may be subjected to high humidity environments, which can cause the delivery system to be unstable during storage.

[0005] In flavor delivery systems, waterproof or moisture-insensitive materials are rarely considered. Examples of such materials include condensate core-shell microcapsules, which release flavor upon mechanical rupture. However, this system is limited by the range of active substances that can be encapsulated based on their polarity.

[0006] In most solid delivery systems (such as spray drying and extrusion), flavoring molecules are entrapped within an amorphous, glassy matrix of a carrier, typically a starch hydrolysate. The release mechanism is primarily based on dissolution, which makes these systems sensitive to moisture. A common solution to improve the moisture stability of such delivery systems is to increase the molecular weight of the carrier system, but this has limitations in terms of viscosity and barrier properties. Another method to improve the moisture stability of solid delivery systems is to coat them with a hydrophobic layer. This coating is typically achieved by using a fluidized bed or roller-jet spraying of molten solid fats, thus requiring additional process steps.

[0007] Therefore, it is desirable to provide extruded granules with enhanced moisture stability that can be prepared by a simple method.

[0008] The present invention provides a method for solving the above-mentioned problems. Summary of the Invention

[0009] It has been surprisingly discovered that particles with a hydrophobic coating (made from solid fat) can be obtained by extrusion without additional steps. In fact, when solid fat is added to a conventional formulation (i.e., a mixture of carrier material and active ingredient such as flavor oil), the fat undergoes phase separation according to temperature in the process, and as the molten material is exchanged into smaller entities in the cutting step, the fat solidifies on the particle surface, thus forming a hydrophobic coating.

[0010] Therefore, the first object of the present invention is a method for preparing extruded granules, comprising the following steps:

[0011] a) Mix at least one carrier material and a plasticizer, preferably water, to form a mixture;

[0012] b) Heat the mixture at a temperature sufficient to form a molten substance;

[0013] c) The molten material is extruded through a die to form an extrudate;

[0014] d) Cut the extrudate to form extruded pellets.

[0015] Solid fats having a melting point Tm and active ingredients, preferably containing flavoring agents (seasonings / food flavorings) or perfumes (floral fragrances), are added to the mixture in step a) and / or the molten material in step b).

[0016] At least steps c) and d) are performed at temperatures above Tm.

[0017] Unless otherwise stated, percentages (%) are intended to specify a weight percentage of the composition.

[0018] The phrase “at least steps c) and d) are carried out at temperatures above Tm” should be understood to mean that the molten material in step c) and the extrudate in step d) have temperatures above Tm.

[0019] In one particular implementation, the particles are amorphous particles.

[0020] In one particular embodiment, the glass transition temperature of the particles is equal to or greater than 25°C, preferably equal to or greater than 30°C, and more preferably equal to or greater than 40°C. In one particular embodiment, the glass transition temperature of the flavoring particles is preferably equal to or less than 120°C, preferably equal to or less than 100°C, and more preferably equal to or less than 90°C. In one particular embodiment, the glass transition temperature of the flavoring particles is greater than 25°C and less than 120°C, preferably greater than 35°C and less than 100°C, and more preferably 40°C to 90°C. The glass transition temperature can be measured by standard methods known to those skilled in the art, for example, using a differential scanning calorimeter DSC822e (Mettler).

[0021] In one particular implementation, the particles are in a solid, particulate state.

[0022] In one particular implementation, the particles are free-flowing.

[0023] In one particular embodiment, the average particle size is equal to or greater than 300 μm, and preferably equal to or greater than 500 μm. In one particular embodiment, the average particle size of the flavoring particles is equal to or less than 1 cm, preferably equal to or less than 5 mm, and more preferably equal to or less than 3 mm. In one particular embodiment, the average particle size of the flavoring particles is preferably 300 to 10000 μm, more preferably 500 to 3000 μm. The average particle size can be measured by standard methods known to those skilled in the art, for example, using a Beckman Coulter laser diffraction particle size analyzer (Coulter LS 13320) equipped with a Tornado Dry Powder Module (Beckman Coulter Inc., Miami, FL). The average particle size can also be determined by sieving.

[0024] The carrier material in step a) can be any compound that can be easily processed by extrusion technology to form a dry extruded solid.

[0025] In one particular implementation, the carrier material in step a) is actually neutral from the perspective of flavoring agents, i.e., it does not significantly alter the sensory properties of the flavoring ingredients.

[0026] In one particular implementation, the carrier material in step a) is a solid carrier.

[0027] In one particular implementation, the carrier material in step a) is a biopolymer.

[0028] Biopolymers can be defined as chain-like molecules composed of repeating chemical blocks derived from renewable resources that can degrade in the environment.

[0029] In one particular implementation, the carrier material in step a) is a food-grade biopolymer.

[0030] In one particular implementation, the carrier material in step a) is a water-soluble food-grade biopolymer. Water-soluble food-grade biopolymers typically comprise macromolecules (including proteins, nucleic acids, and polysaccharides) formed from living organisms.

[0031] In one particular implementation, the carrier material in step a) is a starch derivative, gum, fiber, polysaccharide, protein, soluble flour, or a mixture thereof.

[0032] The term "starch derivative" has its normal meaning to those skilled in the art. Starch derivatives are prepared by altering the properties of natural starch through enzymatic, physical, or chemical treatment.

[0033] The term "hydrolyzed starch" refers to oligosaccharide materials typically obtained by acid and / or enzymatic hydrolysis of starch, preferably corn starch.

[0034] According to one particular implementation, hydrolyzed starch is selected from the group consisting of maltodextrin, dextrin, corn syrup, and mixtures thereof.

[0035] According to one particular implementation scheme, the carrier material also includes modified starch.

[0036] The term "modified starch" has the normal meaning to those skilled in the art, that is, starch that has been modified by physical means (physical modification), enzymatic means (enzymatic modification), or chemical means (chemical modification).

[0037] "Physically modified starch" refers to starch that has undergone heat treatment in the presence of relatively small amounts of water or moisture. No other reagents are added to the starch during the heat treatment process. The heat treatment process includes wet heat treatment and annealing, both of which cause physical modification of the starch without gelatinization.

[0038] "Enzyme-modified starch" refers to starch that has been treated with one or more enzymes to change its properties.

[0039] "Chemically modified starch" refers to starch that has been reacted with reagents added to starch to form new covalent bonds between those molecules and starch molecules.

[0040] Specific examples of modified starches include hydroxypropyl starch, phosphate starch phosphate, octenyl succinate starch, octenyl succinate starch aluminum, acetylated distarch phosphate, acetylated distarch adipate, acetylated distarch adipate, hydroxypropyl distarch phosphate, and acetylated oxidized starch. Some non-limiting examples include octenyl succinic anhydride modified starch, such as Tate & Lyle's... Ingredion Cargill wait.

[0041] Specific examples of starch derivatives include maltodextrin, dextrin, resistant starch, hydroxypropyl starch, phosphate starch phosphate, octenyl succinate starch, octenyl succinate starch aluminum, acetylated distarch phosphate, acetylated distarch adipate, acetylated distarch adipate, hydroxypropyl distarch phosphate, and acetylated oxidized starch.

[0042] The term "gum" has its normal meaning to those skilled in the art. Gum can be derived from plant sources, seaweed, and bacterial fermentation. Specific examples of gum include gum arabic, gum tragacanth, gum karaya, gum ghatti, ocra gum, glucomannan, gellan gum, alginate, etc. The term "fiber" has its normal meaning to those skilled in the art. Fibers cannot be digested by human enzymes. Specific examples of fiber include inulin, fructooligosaccharides, β-glucan, arabinogalactan, glucomannan, psyllium, soluble corn fiber, etc. The term "polysaccharide" has its normal meaning to those skilled in the art. Specific examples of polysaccharides include tamarind seed polysaccharide, soybean polysaccharide, galactomannan, xyloglucan, carrageenan, pectin, curdlan, arabinogalactan, arabinogalactan, etc. The term "protein" has its normal meaning to those skilled in the art. Specific examples of proteins include pea protein, soy protein, lentil protein, chickpea protein, rice protein, potato protein, broad bean protein, mung bean protein, and low-erucic acid rapeseed (canola) protein. The term "soluble flour" has its normal meaning to those skilled in the art. Soluble flour is flour that has undergone chemical, physical, or enzymatic treatment to increase its solubility and functionality. Specific examples of soluble flour include soluble rice flour, soluble brown rice flour, and koji rice.

[0043] In one particular embodiment, the carrier material comprises maltodextrin with a dextran equivalent (DE) of about 1 to about 20.

[0044] In one particular embodiment, the maltodextrin is selected from maltodextrin with a DE of about 10 to about 18 DE.

[0045] In another embodiment, the carrier material comprises corn syrup with a DE of 21 to 49. Any carrier material can be used, made by hydrolyzing starch from various sources (e.g., but not limited to, corn, wheat, potatoes, or rice). In another embodiment, the carrier material is hydrogenated starch hydrolysate (e.g., HSPolyols), fructose oligosaccharides (e.g., but not limited to inulin from Orafit), soluble fiber such as, but not limited to, Nutriose (Roquette), and pregelatinized starch.

[0046] The glass transition temperature of the mixture of active material (e.g., flavoring agent) and carrier depends on the amount of plasticizer added to the initial mixture.

[0047] According to one embodiment, the glass transition temperature of the particles is substantially the same as that of the mixture. This is achieved by ensuring minimal or no water loss.

[0048] According to this particular embodiment, a small amount of plasticizer, preferably water, is added to the mixture to ensure that the glass transition temperature (Tg) of the resulting melt corresponds to and is substantially the same as the desired Tg value of the final product. In other words, unlike other methods such as wet granulation, the glass transition temperature of the mixture before extrusion has already reached the value required for the final product, which is above room temperature, preferably above 40°C, so that the product can be stored at ambient temperature in the form of free-flowing granules. Therefore, this embodiment of the invention eliminates the need for an additional drying step after extrusion, which aims to remove water to raise the Tg to an acceptable value, and thus reduces energy requirements.

[0049] Therefore, the proportion of plasticizer used in this invention varies over a wide range of values, and those skilled in the art can adjust and select these values ​​according to the properties of the carrier and the required Tg of the final product.

[0050] According to one embodiment, the plasticizer content causes the mixture to have a glass transition temperature Tg higher than room temperature.

[0051] Water is the preferred plasticizer, but polyols such as glycerol, propylene glycol, and their esters (i.e., triacetin) can also be used. Small polar molecules can be used to lower Tg, and other examples include organic acids (citric acid, maleic acid, etc.), amino acids, monosaccharides and disaccharides (glucose, maltose, fructose, sucrose, etc.) and mixtures thereof.

[0052] Typically, based on the total weight of the mixture from step a), the amount of plasticizer used is 0.5% to 10%, preferably 5% to 9%.

[0053] In one particular embodiment, a lubricant is provided in step a) and / or step b). While not wishing to be limited to any theory, the lubricant is believed to reduce shear and expansion of the molten material at the exit die. In some embodiments, the lubricant may comprise a medium-chain triglyceride (MCT). In another embodiment, the lubricant comprises a micellar surfactant such as lecithin or a fatty acid ester (e.g., citric acid, tartaric acid, acetic acid), DATEM, CITREM, or a mixture thereof. In one particular embodiment, the lubricant may be provided in an amount of up to about 5% by weight of the total weight of the mixture in step a), particularly about 0.2% to up to about 5%, more particularly about 0.8% to up to about 2%, and even more particularly about 1% to 2%.

[0054] According to a specific embodiment, in step a), a low molecular weight carbohydrate is added, preferably from sucrose, glucose, lactose, maltose, fructose, ribose, dextrose, isomaltitol, sorbitol, mannitol, xylitol, lactitol, maltitol, pentitol, arabinose, glucose syrup, pentose, xylose, galactose, and trehalose. The mixture is selected from the group and is preferably provided in an amount of 1 to 10% by weight, preferably 2 to 6% by weight, based on the total weight of the mixture from step a).

[0055] According to one embodiment, in step a) and / or b), an additional component preferably selected from the group consisting of gums, proteins, small molecule surfactants, plant extracts, saponins, plant-derived proteins, protein hydrolysates, citrus fiber, beet fiber, or mixtures thereof is added, preferably in an amount of 1 to 30% by weight, preferably 5 to 20% by weight, more preferably 10 to 20% by weight (based on the total weight of the flavoring particles, preferably the particles).

[0056] The term "gum" has its normal meaning to those skilled in the art. Specific examples of gums include gum arabic, ark tartaricus gum, solanum, tragali gum, okra gum, etc. The term "protein" has its normal meaning to those skilled in the art. Specific examples of proteins include pea protein, soybean protein, lentil protein, chickpea protein, rice protein, potato protein, broad bean protein, mung bean protein, low-erucic acid rapeseed protein, etc. The term "small molecule surfactant" has its normal meaning to those skilled in the art. Specific examples of small molecule surfactants include saponins from bark trees, saponins from yucca, phospholipids, lecithin, lysophosphatidylcholine, diacetyl tartaric acid and glycerol fatty acid esters (DATEM), glycerol mono- and di-citrate esters (CITREM), etc.

[0057] The mixture from step a) is then heated in an extruder, typically a single-screw extruder, a twin-screw extruder, or a plunger extruder, preferably a twin-screw extruder.

[0058] According to one particular implementation, step a) is performed at a temperature above Tm.

[0059] According to one particular implementation, step b) is performed at a temperature above Tm.

[0060] The mixture from step a) is thus extruded in an extruder that maintains the temperature of the mixture at a predetermined temperature, preferably between 90 and 130°C. This temperature is suitable for the system of the present invention. In practice, it must be higher than the glass transition temperature of the carrier material and also higher than the Tm (melting temperature) of the solid fat in order to keep the mixture in the form of a molten substance. Pressure is also applied and adjusted to a value suitable for maintaining melt homogeneity. Typically, depending on the size of the equipment, up to 100 bar (10) can be used. 7 Pressure value (Pa).

[0061] According to the present invention, an active ingredient (e.g., flavor oil or spice oil) and a solid fat having a melting temperature (typically above room temperature) are added to the mixture in step a) and / or the molten material in step b).

[0062] According to the present invention, the cutting step occurs when the fat is in a liquid state.

[0063] According to one embodiment, the active ingredient is a hydrophilic material. According to another embodiment, the active ingredient is a hydrophobic material.

[0064] According to a preferred embodiment, the active ingredient comprises a flavoring agent or fragrance.

[0065] According to a preferred embodiment, the active ingredient is a flavoring agent or fragrance.

[0066] According to a preferred embodiment, the active ingredient is a flavor oil or fragrance oil.

[0067] According to one implementation scheme, the hydrophobic material is the hydrophobic active ingredient.

[0068] According to one embodiment, the amount of active ingredient added is 1% to 20% based on the weight of the mixture obtained after step a) or step b).

[0069] According to a preferred embodiment, the active ingredient comprises a flavor oil or fragrance oil. Alternative ingredients that may benefit from encapsulation can be used in place of, or in combination with, fragrances or flavorings. Non-limiting examples of such ingredients include cosmetics, skin care products, odor neutralizers, bactericides, fungicides, pharmaceutical or agricultural chemicals, disinfectants, insect repellents or attractants, and mixtures thereof.

[0070] The nature and type of insect repellents or attractants that may exist in the hydrophobic internal phase are not guaranteed to be described in more detail here, and in any case, it is impossible to be exhaustive. Those skilled in the art can select them based on their general knowledge and according to their intended use or application.

[0071] Examples of such insect repellents or attractants include essential oils of birch, DEET (N,N-diethyl-m-toluamide), lemon eucalyptus (Corymbia citriodora) and their active compounds p-menthane-3,8-diol (PMD), icaridin (hydroxyethyl isobutylpiperidine carboxylate), nepelactone, citronella oil, neem oil, Bog Myrtle (Myrica Gale), dimethyl carbate, tricyclodecenyl allyl ether, IR3535 (ethyl 3-[N-butyl-N-acetyl]aminopropionate), ethylhexanediol, dimethyl phthalate, metofluthrin, Indalone, SS220, anthranilate-based insect repellents, and mixtures thereof.

[0072] By "flavor oil," this refers to a flavoring ingredient, or a mixture of multiple flavoring ingredients, solvents, or adjuvants currently used in the preparation of flavor formulations, that is, a specific mixture of components intended to be added to an edible composition or chewable product to impart, improve, or modify its sensory properties, particularly its flavor and / or taste. Flavoring ingredients are well known to those skilled in the art, and their properties are not guaranteed to be described in greater detail herein; in any case, they cannot be exhaustive, and a skilled flavorist is able to select them based on their general knowledge and according to the intended use or application and the desired sensory effects. Many of these flavoring ingredients are listed in references such as S. Arctander's book *Perfume and Flavor Chemicals*, 1969, Montclair, NJ, USA, or its latest edition, or other works of a similar nature, such as Fenaroli's Handbook of Flavor Ingredients, 1975, CRC Press, or MB Jacobs' *Synthetic Food Adjuncts*, 1947, van Nostrand Co., Inc. Solvents and adjuvants currently used in the preparation of flavor formulations are also well known in the art.

[0073] In one particular embodiment, the flavoring agent is a peppermint flavoring agent. In a more specific embodiment, the peppermint is selected from the group consisting of peppermint and spearmint.

[0074] In a further embodiment, the flavoring agent is a cooling agent or a mixture thereof.

[0075] In another embodiment, the flavoring agent is menthol.

[0076] Flavoring agents derived from or based on fruits (in which citric acid is the predominant naturally occurring acid) include, but are not limited to, citrus fruits (e.g., lemons, limes), limonene, strawberries, oranges, and pineapples. In one embodiment, the flavored food is lemon juice, lime juice, or orange juice extracted directly from the fruit. Other embodiments of the flavoring agent include juices or liquids extracted from oranges, lemons, grapefruits, limes, citrons, clementines, mandarins, tangerines, and any other citrus fruits or their varieties or hybrids. In a particular embodiment, the flavoring agent includes liquids extracted or distilled from oranges, lemons, grapefruits, limes, citrons, clementines, mandarins, tangerines, any other citrus fruits or their varieties or hybrids, pomegranates, kiwifruits, watermelons, apples, bananas, blueberries, melons, ginger, bell peppers, cucumbers, passion fruit, mangoes, pears, tomatoes, and strawberries.

[0077] In one particular embodiment, the flavoring agent comprises a composition containing limonene. In another particular embodiment, the composition is a citrus fruit that further contains limonene.

[0078] In another specific implementation, the flavoring agent comprises a flavoring agent selected from the group consisting of strawberry, orange, lime, tropical fruit, berry mixture and pineapple.

[0079] Phrase flavorings include not only flavoring agents that impart or modify the aroma of food, but also components that impart or modify the taste. The latter may not necessarily have a taste or aroma themselves, but can improve the taste provided by other components such as salt-enhancing components, sweet-enhancing components, umami-enhancing components, bitterness-blocking components, etc.

[0080] In a further embodiment, a suitable sweetening component may be included in the particles described herein. In one particular embodiment, the sweetening component is selected from the group consisting of sugars (e.g., but not limited to sucrose), stevia components (e.g., but not limited to steviol glycosides or rebaudioside A), sodium cyclohexylsulfamate (cyclamate), aspartame, sucralose, sodium saccharin, and acesulfame potassium, or mixtures thereof.

[0081] By "fragrance oil" (or "fragrance"), it refers herein to an ingredient or composition that is liquid at about 20°C. The fragrance oil or flavoring oil may be a single flavoring or flavoring ingredient, or a mixture of multiple ingredients in the form of a flavoring or flavoring composition. As a "flavoring ingredient," it refers herein to a compound whose primary purpose is to impart a pleasant effect in a flavoring preparation or composition. In other words, to be considered a flavoring ingredient, such an ingredient must be recognized by those skilled in the art as capable of imparting or modifying the odor of a composition, at least in an active or pleasant manner, and not merely possessing an odor. The nature and type of flavoring ingredients present in the oil phase are not guaranteed to be described in greater detail here, and it is impossible to be exhaustive in any way; those skilled in the art can select them based on their common sense and according to the intended use or application and the desired sensory effect. Generally, these flavoring ingredients belong to different chemical classifications, such as alcohols, aldehydes, ketones, esters, ethers, acetates, nitriles, terpenes, nitrogen- or sulfur-containing heterocyclic compounds, and essential oils, and the flavoring auxiliary ingredients may be of natural or synthetic origin. Many of these auxiliary ingredients are listed in references such as S. Arctander's *Perfume and Flavor Chemicals*, 1969, Montclair, New Jersey, USA, or later editions thereof, or other works of a similar nature, as well as in the extensive patent literature within the fragrance industry. It should also be understood that the ingredients may also be compounds known to release various types of flavoring compounds in a controlled manner.

[0082] For active ingredients in solid form, the addition in step a) is more appropriate, while for active ingredients in liquid form (e.g., flavor oil), the addition in step b) is more appropriate.

[0083] According to a specific implementation scheme, an active ingredient (e.g., flavor oil) is added in step a).

[0084] According to a specific implementation scheme, an active ingredient (e.g., flavor oil) is added in step b).

[0085] As used in this invention, the term "fat" refers to a lipid component that is in solid or paste form at room temperature (typically 20°C to 30°C, more specifically 25°C), while the term "oil" refers to a lipid component that is liquid at room temperature. It should be understood that fats can be in solid or liquid state depending on the temperature during different steps of the process.

[0086] Those skilled in the art will be able to select a suitable solid fat based on its melting point. According to the invention, the solid fat has a melting point (Tm) above room temperature.

[0087] The melting point (Tm) of a material can be readily determined by those skilled in the art or found in the literature. The melting point can be measured using differential scanning calorimetry (DSC). A typical method is as follows: measurements are performed on a Mettler-Toledo DSC822e in a 40 μL aluminum crucible. The sample is held at -10 °C for 2 minutes, and the temperature is increased to 150 °C at a rate of 10 °C / min. The melting characteristic is a distinct endothermic peak, the apex of which represents the melting point temperature.

[0088] Among suitable fats that can be used in this invention, non-limiting examples include beeswax, candelilla wax, carnauba wax, paraffin wax, palm fat, shea butter, algae butter, hydrogenated vegetable oil, palm stearin, shea butter stearin, rice stearin, sunflower stearin, animal fat, cocoa butter, saturated fatty acids (e.g., lauric acid, myristic acid, palmitic acid, stearic acid, arachidic acid and their corresponding monoglycerides, diglycerides and triglycerides with melting points above room temperature), and mixtures thereof.

[0089] According to one embodiment, the melting temperature of fat is in the range of 30 to 90°C. According to another embodiment, the melting temperature of fat is in the range of 40 to 90°C. According to yet another embodiment, the melting temperature of fat is in the range of 50 to 90°C.

[0090] The surface area of ​​the fat-covered particles is related to the square of the particle size. Therefore, those skilled in the art will be able to adapt the amount of solid fat to the desired particle size.

[0091] According to one embodiment, based on a carrier system composed of a carrier material and solid fat, the amount of solid fat is 0.5 to 30% by weight, preferably 1 to 10% by weight.

[0092] According to one embodiment, when the mixture reaches the die section of the extruder, the temperature is still above the glass transition temperature of the carrier and also above the Tm of the solid fat. The extruder is equipped with a die cutter, so the mixture is cut at the melt temperature. Once cooled to ambient temperature, the cut glass material does not need to be shaped or dried in a rounding mill, fluidized bed dryer, or other equipment, unlike other processes that cool the molten carrier before cutting. In one particular embodiment, the ambient air includes cold air.

[0093] According to one embodiment, the method includes an additional step between step b) and step c) of pumping the molten material and propelling the molten material through a static mixer. The pumping step can be performed using a gear pump, preferably a polymer gear pump, which allows the melt to be removed from the extruder and propelled through the static mixer, or it can be accomplished solely by the action of the twin-screw extruder itself.

[0094] In the extrusion process, the mixture is forced through a die with an orifice of a predetermined diameter, which typically ranges from about 0.250 to 10 mm, more particularly from about 0.5 to about 3.0 mm, and even more particularly from 0.7 to 3.0 mm. However, much larger die diameters are also possible.

[0095] In one particular implementation, an extruder such as, but not limited to, Thermo Prism 16mm twin-screw laboratory extruder or Clextral BC21, equipped with a cutter blade, can be used to granulate the melt at the die exit.

[0096] Typically, an extruder barrel consists of multiple barrel sections, each with independently temperature-controlled components. In one embodiment, the extruder includes 2 to 9 heating and cooling zones with a temperature range of approximately 20 to 120°C.

[0097] Another object of the present invention is extruded pellets that can be obtained by the method defined above.

[0098] According to one embodiment, the extruded pellets comprise:

[0099] - Active ingredients, preferably flavorings or fragrances dispersed in a matrix made of a carrier material, and

[0100] - A coating containing solid fats.

[0101] It should be understood that the particles of the present invention contain a hydrophobic coating (i.e., made of solid fat).

[0102] According to a specific implementation scheme, the particle size is greater than 300 micrometers, preferably greater than 500 micrometers.

[0103] It has been shown that the presence of the hydrophobic coating provides enhanced moisture stability. In fact, according to one embodiment, the extruded particles exhibit enhanced moisture stability because they maintain their integrity at 80% relative humidity and 25°C. No visual collapse or melting was observed under these conditions.

[0104] The granules of this invention can be used in a variety of edible end products.

[0105] Therefore, another object of the present invention is flavored or scented consumer products comprising extruded particles as defined above.

[0106] "Consumer goods" or "final products" refer to manufactured goods that are ready for distribution, sale, and use by consumers.

[0107] Flavored consumer products

[0108] The final products are more specifically food, pet food, or feed products.

[0109] Because the particles of this invention contain a hydrophobic coating, they are particularly advantageous for dried foods that are susceptible to rehydration, such as instant beverages (PSD, chocolate, coffee), confectionery such as chewing gum, instant noodles, or soup cubes.

[0110] The particles of this invention are particularly advantageous for foods with relatively high water activity, such as ready-to-eat meals, meat analogues, microwaveable foods, and pasta boxes.

[0111] The granules of this invention can be used in vegetarian meat analogues or meat substitutes, vegetarian burgers, sausages, patties, imitation chicken nuggets, etc., meat products (e.g., processed meats, poultry, beef, pork, ham, fresh sausages or raw meat products, fresh meat marinated with spices or acid or cured meat products, reformed meat), or extended meat products using different proportions of animal and plant protein combinations, typically co-extruded or obtained by mixing textured plant protein and animal protein.

[0112] For the purposes of this invention, meat includes red meat, such as beef, pork, mutton, lamb, game, and poultry, such as chicken, turkey, goose, and duck. Preferably, the food of this invention is meat selected from beef, poultry, and pork.

[0113] However, the particles of the present invention may also be of particular interest in examples of the following products:

[0114] • Baked goods (such as bread, dry biscuits, cakes, and other baked goods),

[0115] • Non-alcoholic beverages (such as carbonated soft drinks, bottled water, sports / energy drinks, fruit juices, vegetable juices, and vegetable juice preparations),

[0116] • Alcoholic beverages (such as beer and malt drinks, spirits),

[0117] • Instant beverages (such as instant vegetable drinks, powdered soft drinks, instant coffee and tea),

[0118] • Cereal products (such as breakfast cereals, pre-cooked ready-made rice products, rice flour products, millet and sorghum products, raw or pre-cooked noodles and pasta products),

[0119] Dairy products (such as fresh cheese, soft cheese, hard cheese, milk beverages, whey, butter, partially or completely hydrolyzed milk protein products, fermented dairy products, condensed milk and the like),

[0120] Dairy products (such as fruit or flavored yogurt, ice cream, fruit shaved ice, frozen desserts),

[0121] • Confectionery products (such as chewing gum, hard candy, and soft candy)

[0122] Chocolate and compound coatings

[0123] • Products based on fats and oils or their emulsions (e.g., mayonnaise, spreads, margarine, shortening, remoulade, dressings, flavored preparations),

[0124] Spiced, marinated, or processed fish products (such as fish intestines, fish paste),

[0125] • Eggs or egg products (dried eggs, egg whites, egg yolks, custards)

[0126] • Desserts (such as gelatin and pudding)

[0127] Products made from soy protein or other soy components (such as soy milk and products made therefrom, preparations containing soy lecithin, fermented products such as tofu or tempeh or products made therefrom, soy sauce),

[0128] • Vegetable products (e.g., tomato sauce, dressings, processed and reconstituted vegetables, dried vegetables, deep-frozen vegetables, pre-cooked vegetables, pickled vegetables, vegetable concentrates or pastes, cooked vegetables, potato products),

[0129] Vegetarian meat alternatives, vegan burgers

[0130] Spices or spice products (such as mustard products, horseradish products), spice blends, especially seasonings used in the snack industry.

[0131] • Snacks (such as baked or fried potato chips or potato dough products, bread dough products, extrusions based on corn, rice, or chopped nuts),

[0132] • Meat products (such as processed meats, poultry, beef, pork, ham, fresh sausages or raw meat products, fresh meat marinated with spices or acid or cured meat products, and reformed meat),

[0133] • Ready-to-eat dishes (such as instant noodles, rice, pasta, pizza, tortillas, wraps) as well as broths and stock (such as stock, savory cube, dry stock, instant stock, pre-cooked stock, distilled stock) and sauces (instant sauce, dry sauce, prepared sauce, gravy, sweet sauce).

[0134] Preferably, the granules according to the invention are applied to products selected from the group consisting of: baked goods, instant beverages, cereal products, dairy products, milk products, fat and oil-based products or emulsions thereof, desserts, vegetable products, vegetarian meat substitutes, spices and seasonings, snacks, meat products, ready-to-eat dishes, broths and stock, and sauces.

[0135] According to one particular implementation, the flavored product is selected from the group consisting of: meat and / or fish products or similar, broth bases, bulk soup bases, powder mixtures, beef or pork products, seafood, surimi, instant noodles, rice, soup, sauces, ready-to-eat meals, frozen or chilled pizzas, pasta, potato chips or fried potatoes, noodles, potato chips / corn chips, microwave popcorn, nuts, pretzels, rice cakes, rice cakes, fermented dairy product analogues, acidified dairy product analogues, non-fermented dairy product analogues, cheese or cheese analogues, yogurt or yogurt analogues, nutritional supplements, nutrition bars, cereals, ice cream, dairy-free ice cream, confectionery products, chewing gum, hard candy, and powdered beverages.

[0136] According to one embodiment, food, pet food, or feed products contain 0.01 to 10% by weight, preferably 0.1 to 5% by weight, of the particles of the present invention.

[0137] Typically, food, pet food, or feed products also contain protein, especially plant or animal protein, as well as mixtures thereof.

[0138] Advantageously, the plant protein is preferably selected from soybean protein, corn, peas, low-erucic acid rapeseed, sunflower, sorghum, rice, amaranth, potato, cassava, kudzu root, chickpea, lupin, low-erucic acid rapeseed, wheat, oats, rye, barley, and mixtures thereof.

[0139] The granules of this invention are particularly suitable for extruded and / or baked food, pet food, or feed products, more particularly containing animal and / or plant proteins. Typically, the extruded and / or baked food, pet food, or feed products may be selected from meat and / or fish foods or their analogues and mixtures (in other words, meat and / or fish foods or meat analogues or fish analogues and mixtures thereof); extruded and / or baked meat analogues or extruded and / or baked fish analogues are preferred. Non-limiting examples of extruded and / or baked food, pet food, or feed products are snack products or extruded plant proteins intended to give texture to proteins used in the preparation of meat analogues (e.g., hamburgers). Powdered compositions may be added before or after extrusion to non-extruded plant protein isolates / concentrates or textured plant proteins that can form hamburgers or meat chunks (etc.).

[0140] Scented consumer products

[0141] The particles of the present invention can be used in combination with active ingredients. Therefore, one object of the present invention is a composition comprising:

[0142] (i) Particles as defined above;

[0143] (ii) Active ingredients, preferably selected from the group consisting of: cosmetic ingredients, skin care ingredients, fragrance ingredients, flavoring ingredients, odor-dispelling ingredients, bactericide ingredients, fungicide ingredients, pharmaceutical or agricultural chemical ingredients, disinfectant ingredients, insect repellents or attractants, and mixtures thereof.

[0144] The particles of this invention can also be added to various flavored consumer products.

[0145] The granules can be used in powder form suitable for powdered consumer products.

[0146] When the particles comprise a fragrance oil-based core, the products of the present invention are particularly suitable for use in scented consumer products, such as those belonging to high-quality fragrances or "functional" fragrances. Functional fragrances particularly include personal care products, including hair care, body cleansing, skin care, hygiene care, and home care products, including clothing care and air care. Therefore, another object of the present invention is a scented consumer product comprising the aforementioned particles as a fragrance ingredient.

[0147] In addition, the following powdered consumer products are also part of this invention, comprising:

[0148] - At least one surfactant comprising 2 to 65% by weight of the total weight of the consumer product; and

[0149] - Particles as defined above, wherein the active ingredient contains fragrances as defined above.

[0150] Furthermore, the following liquid consumer products are part of this invention, comprising:

[0151] - At least one surfactant comprising 2 to 65% by weight of the total weight of the consumer product; and

[0152] - Particles as defined above, wherein the active ingredient contains fragrances as defined above.

[0153] For clarity, it must be mentioned that "fragrant consumer product" refers to a consumer product intended to deliver the fragrance effect, among various benefits, to surfaces to which it is applied (e.g., skin, hair, fabric, paper, or household surfaces) or into the air (air fresheners, deodorants, etc.). In other words, the fragrant consumer product according to the invention is a processed product comprising a functional formulation (also referred to as a "base") and beneficial agents, wherein an effective amount of particles according to the invention is contained.

[0154] Another object of the present invention is a consumer product comprising:

[0155] - Personal care active base, and

[0156] -Particles as defined above or flavored compositions as defined above

[0157] Consumer products are in the form of personal care compositions.

[0158] Personal care active base materials incorporating the particles of this invention can be found in a large body of literature relating to this product. These formulations are not guaranteed to be described in detail here, and are by no means exhaustive. Those skilled in the art of formulating such consumer products are fully capable of selecting appropriate components based on their general knowledge and available literature.

[0159] Personal care compositions are preferably selected from the group consisting of: hair care products (e.g., dry shampoo, hair spray), cosmetic preparations (e.g., cold cream, body lotion, or deodorant or antiperspirant), or skin care products (e.g., soap, bath salts, or hygiene products), and oral care products (toothpaste or mouthwash compositions).

[0160] Another object of the present invention is a consumer product comprising:

[0161] - Active base materials for home care or fabric care, and

[0162] -Particles as defined above or flavored compositions as defined above

[0163] The consumer products are in the form of home care or fabric care compositions.

[0164] Numerous documents relating to this product can be found on home care or fabric care bases in which the particles of this invention can be incorporated. These formulations are not guaranteed to be described in detail here, and are by no means exhaustive. Those skilled in the art of formulating such consumer products are fully capable of selecting appropriate components based on their general knowledge and available literature.

[0165] Home or fabric care compositions are preferably selected from powdered detergents and solid fragrance enhancers. Detailed Implementation

[0166] Example

[0167] Example 1

[0168] Preparation of extruded particles (particle A) according to the method of the present invention

[0169] Weigh all ingredients in the table below and mix them in a mixing bowl, starting with the solids and adding water last. Then extrude the mixture using a 16mm laboratory extruder from Thermo Electron (Germany). Extrusion parameters are as follows: feeder throughput 400g / h, die temperature 110°C, 4 barrel sections with a temperature range of 20°C to 110°C. Die orifice inner diameter is 1mm. Screw speed is set to 300rpm.

[0170] 20 <![CDATA[Carnauba wax 1) > 35 water 2.5 <![CDATA[lecithin 2) > 420 <![CDATA[Maltodextrin 6DE 3) > 2.5 <![CDATA[NEOBEE 4) ]]> 40 Coffee flavoring

[0171] 1) Source: Kahlwax

[0172] 2) Source: Lasenor

[0173] 3) Source: Roquette

[0174] 4) Source: Stepan

[0175] After establishing steady-state extrusion conditions (the melting temperature of the extrudate is 93°C), the extrudate is cut into approximately 1.5 mm particles using a rotary cutter and collected by a cyclone separator.

[0176] Comparative Example 2

[0177] Comparative preparation of extruded granules (granules X)

[0178] Weigh all ingredients in the table below and mix them in a mixing bowl, starting with the solids and adding water last. Then extrude the mixture using a 16mm laboratory extruder from Thermo Electron (Germany). Extrusion parameters are as follows: feeder throughput 400g / h, die temperature 110°C, 4 barrel sections with a temperature range of 20°C to 110°C. Die orifice inner diameter is 1mm. Screw speed is set to 300rpm.

[0179] 35 water 2.5 <![CDATA[lecithin 1) > 420 <![CDATA[Maltodextrin 6DE 2) > 2.5 <![CDATA[NEOBEE 3) ]]> 40 Coffee flavoring

[0180] 1) Source: Lasenor

[0181] 2) Source: Roquette

[0182] 3) Source: Stepan

[0183] After establishing steady-state extrusion conditions (the melting temperature of the extrudate is 93°C), the extrudate is cut into approximately 1.5 mm particles using a rotary cutter and collected by a cyclone separator.

[0184] Example 3

[0185] Water solubility assessment (particle A compared to control particle X)

[0186] Differences in water solubility were assessed by placing particles A (Example 1) and particles X (Comparative Example 2) according to the invention side-by-side under a microscope. Deionized water was added between glass plates to track their dissolution, magnified 4 times.

[0187] It has been observed that particle X dissolves in water more quickly than particle A of the present invention, indicating that the hydrophobic coating present on the surface of the particles of the present invention protects the particles under humid conditions.

[0188] Example 4

[0189] Preparation of extruded particles (particles C to I) according to the method of the present invention

[0190] First, the solid fat and flavoring agent were mixed together and heated at 80°C to obtain a homogeneous liquid. After cooling, the solid fat phase was mixed with the remaining ingredients in a mixing bowl, starting with the solid components and adding water last. The mixture was then extruded using a 16mm laboratory extruder from Thermo Electron (Germany). The extrusion parameters were as follows: feeder throughput 400g / h, die temperature 110°C, 4 barrel sections with a temperature range of 20°C to 110°C, die orifice inner diameter 1mm, and screw speed set to 300rpm.

[0191] <![CDATA[Maltodextrin 18DE 1) > 71 66.2 75 79.5 67.5 84 71 <![CDATA[Modified starch 2) (OSS)]]> 7 7 8 0 7 0 8 <![CDATA[Lecithin 3) > 1 1 1 0 0 0 0 Lemon flavoring 6 6 6 6 6 6 6 <![CDATA[Carnauba wax 4) > 10 15 0 0 0 0 0 <![CDATA[Beeswax 4) > 0 0 5 10 15 0 0 <![CDATA[Hydrogenated soybean glyceride 5) > 0 0 0 0 0 5 10 water 5 4.8 5 4.5 4.5 5 5 100 100 100 100 100 100 100 Moisture sensitivity -- --- - -- --- - ---

[0192] 1) Source: Roquette

[0193] 2) Source: Ingredion

[0194] 3) Source: Lasenor

[0195] 4) Source: Kahlwax

[0196] 5) S-113, Source: Cargill

[0197] For samples C to I, after establishing steady-state extrusion conditions (melting temperature of the extrudate was 99°C), the extrudate was cut into separate particles of approximately 1.5 mm using a rotary cutter and collected via a cyclone separator. All samples exhibited good stability under humid conditions.

Claims

1. A method for preparing extruded granules, comprising the following steps: a) Mix at least one carrier material and a plasticizer to form a mixture; b) Heat the mixture at a temperature sufficient to form a molten substance; c) The molten material is extruded through a die to form an extrudate; d) Cut the extrudate to form extruded pellets. Solid fats having a melting point Tm and active ingredients containing flavorings or fragrances are added to the mixture in step a) and / or the molten material in step b). At least steps c) and d) are performed at temperatures above Tm. The melting temperature range of this solid fat is 30 to 90°C, and The solid fat is selected from the group consisting of: beeswax, candelilla wax, carnauba wax, palm fat, shea butter, microalgae butter, hydrogenated vegetable oil, rice stearin, sunflower stearin, animal fat, cocoa butter, saturated fatty acids, and mixtures thereof. The plasticizer is selected from the group consisting of: water, polyols, organic acids, amino acids, monosaccharides and disaccharides, and mixtures thereof.

2. The method of claim 1, wherein the plasticizer is water.

3. The method of claim 1, wherein the solid fat is palm stearin or shea butter stearin.

4. The method of claim 1, wherein the amount of solid fat is 0.5 to 30% by weight, based on a carrier system composed of a carrier material and solid fat.

5. The method of claim 4, wherein the amount of solid fat is 1 to 10 by weight, based on a carrier system composed of a carrier material and solid fat.

6. The method of claim 1, wherein the carrier material is selected from the group consisting of starch derivatives, gums, fibers, proteins, soluble flours, and mixtures thereof.

7. The method according to claim 1, wherein the carrier material is a polysaccharide.

8. The method according to claim 6, wherein the carrier material is selected from the group consisting of: maltodextrin, resistant starch, hydroxypropyl starch, phosphate starch ester, octenyl succinate starch, acetylated distarch phosphate, acetylated distarch adipate, acetylated oxidized starch, gum arabic, tragacanth gum, ark tartar gum, solanum, glucomannan, gellan gum, alginate, inulin, fructooligosaccharides, β-glucan, arabinogalactan, psyllium husk, soluble corn fiber, tamarind seed polysaccharide, soybean polysaccharide, galactomannan, xyloglucan, carrageenan, pectin, gel polysaccharide, arabinogalactan, pea protein, soybean protein, lentil protein, chickpea protein, rice protein, potato protein, broad bean protein, mung bean protein, low erucic acid rapeseed protein, soluble rice flour, rice koji, and mixtures thereof.

9. The method according to claim 6, wherein the carrier material is dextrin, hydroxypropyl distarch phosphate, or soluble brown rice flour.

10. The method according to any one of claims 1 to 9, wherein a lubricant is added in step a).

11. The method according to any one of claims 1 to 9, wherein in step a) a carbohydrate selected from the group consisting of: sucrose, glucose, lactose, maltose, fructose, ribose, isomaltitol, sorbitol, glucose syrup, mannitol, xylitol, lactitol, maltitol, arabinose, pentose, galactose, trehalose, and mixtures thereof are added.

12. The method of claim 11, wherein the carbohydrate is xylose.

13. Extruded granules obtainable by the method of any one of claims 1 to 12, comprising: - Active ingredients, comprising flavorings or fragrances dispersed in a matrix made of a carrier material, and - A coating containing solid fats.

14. The extruded particles according to claim 13, wherein the particle size is greater than 300 micrometers.

15. The extruded particles according to claim 14, wherein the particle size is greater than 500 micrometers.

16. The extruded granules according to claim 13, 14 or 15, wherein, based on the total weight of the granules, they contain 1 to 20% by weight of a flavoring agent.

17. A food consumer product comprising extruded granules as claimed in any one of claims 13 to 16.

18. A beverage consumer product comprising extruded granules as described in any one of claims 13 to 16.

Citation Information

Patent Citations

  • Microencapsulation of bioactive substances and methods of making the same

    CN102427740A

  • High load flavor particles

    CN109195456A