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    • 专利摘要:
    co-rubbed stabilizing composition, food, industrial composition, and method for making the stabilizing composition. the present invention is directed to a co-rubbed stabilizing composition comprising: (i) microcrystalline cellulose and (ii) carboxymethyl cellulose, wherein the carboxymethyl cellulose has a degree of substitution of about 0.95 - 1.5 and a viscosity of less than 100 cps. the composition is useful as a stabilizer, particularly in food and pharmaceutical applications.
    公开号:BR112014013792B1
    申请号:R112014013792-7
    申请日:2012-11-30
    公开日:2020-09-15
    发明作者:Zheng Tan；Aaron Chip Venables；Michael SESTRICK；Nadia Yaranossian；Jeremy Ondov
    申请人:Dupont Nutrition Usa, Inc；
    IPC主号:
    专利说明:

    FIELD OF THE INVENTION
    [0001] The present invention is directed to co-restricted stabilizer compositions that are suitable for use in, for example, aqueous food and pharmaceutical compositions, their manufacture and use. BACKGROUND OF THE INVENTION
    [0002] Microcrystalline cellulose, also known and referred to here as "MCC", moist cake from hydrolyzed cellulose, or cellulose gel, is commonly used in the food industry to enhance the properties or attributes of a final food product. For example, it has been used as a binder and stabilizer in food applications, including beverages, as a gelling agent, a thickener, a fat substitute, and / or texturizer. It has also been used as a binder and disintegrant in pharmaceutical tablets, as a suspending agent in liquid pharmaceutical formulations, and as a binder, disintegrant and processing aid in industrial applications, in household products such as detergent and / or bleaching tablets, in agricultural formulations, and in personal care products such as toothpaste and cosmetics.
    [0003] Microcrystalline cellulose is modified for such uses by subjecting microcrystalline cellulose or "wet cake" to friction processes to substantially subdivide crystallites into finely divided particles. However, as the particle size is reduced, the individual particles tend to agglomerate or keratinize under drying, a result that is undesirable in product manufacture or use. To prevent keratinization, a protective colloid can be added during friction or following friction but before drying. The protective colloid totally or partially neutralizes hydrogen or other bonding forces between the smaller sized particles. The resulting materials are often referred to as rubbed microcrystalline cellulose or colloidal microcrystalline cellulose and such rubbed or colloidal microcrystalline cellulose will typically form stable suspensions with little or no precipitate. In contrast, non-colloidal microcrystalline cellulose will precipitate and will not form a stable suspension in aqueous systems. Colloidal microcrystalline cellulose, such as microcrystalline cellulose coated with carboxymethyl cellulose, is described in U.S. Patent 3,539,365 (Durand, et al). Another colloidal microcrystalline cellulose, such as starch-coated microcrystalline cellulose, is described in US Patent Application 2011/0151097 (Tuason et al). FMC Corporation (Philadelphia, PA, USA) manufactures and sells various colloidal microcrystalline cellulose products, including edible food and pharmaceutical grades, under the names of, among others, AVICEL® and GELSTAR®.
    [0004] MCC mixtures and some hydrocolloids (such as carboxymethyl cellulose having a degree of substitution of at least 0.95, pectin, alginate, carrageenan, xanthan gum, agar gum, wellan gum, or gellan gum) can be very “slippery ”To be rubbed satisfactorily. Less than satisfactory friction of the MCC particles can have a detrimental effect on the functionality of the MCC stabilizer. As a result, some attempts have been made to solve this problem using a friction agent, for example, a salt. For example, see U.S. 7,897,382, U.S. 7,462,232 and U.S. 5,366,724. Other approaches have been taken to make the MCC / hydrocolloid compositions suitable. For example, see U.S. 2005/0233046, U.S. 2011/0151097, and W02010 / 136157.
    [0005] There remains a need, however, for a co-rubbed colloidal microcrystalline cellulose composition containing a carboxymethyl cellulose having a degree of substitution of at least 0.95 (such carboxymethyl celluloses being slippery). Depositors unexpectedly found that using a carboxymethyl cellulose having a substitution degree of 0.95 - 1.5 and a viscosity of less than 100 mPa.s (100 cps) is capable of being co-rubbed with MCC and that such a stabilizing composition co-rubbing provides superior stabilization in, for example, aqueous food systems. SUMMARY OF THE INVENTION
    [0006] The present invention is directed to a co-attracted stabilizing composition comprising: (i) microcrystalline cellulose and (ii) carboxymethyl cellulose, in which carboxymethyl cellulose has a degree of substitution of 0.95 - 1.5 and a viscosity less than 100 mPa.s (100 cps). The composition is useful as a stabilizer, particularly in food and pharmaceutical applications.
    [0007] The present invention is also directed to an industrial composition comprising the stabilizer of the present invention, wherein the industrial composition is, for example, a pharmaceutical composition, veterinary composition, agricultural composition, or cosmetic composition.
    [0008] In addition, the present invention is directed to a method for making the stabilizing composition of the invention, comprising: a) mixing the microcrystalline cellulose and carboxymethyl cellulose of component (ii); b) co-rubbing the mixture from step a); and c) drying the extrudate from step b). DETAILED DESCRIPTION OF THE INVENTION
    [0009] "Colloid" and "colloidal" are used interchangeably in the present specification to define particles that are capable of being properly suspended in an aqueous mixture. As known to those of ordinary skill in the art and referred to herein, colloidal particles can be of any suitable particle size, provided that they are capable of forming uniform suspensions, eg when measured in suspension, a majority of the particles may have a particle size of 0.1 to 30 microns.
    [0010] All viscosities of the carboxymethyl celluloses referred to here can be measured as follows. The carboxymethyl cellulose used in the present invention is a low viscosity carboxymethyl cellulose having a degree of substitution of 0.95 - 1.5 and a viscosity of less than 100 mPa.s (100 cps). Viscosity of less than 100 mPa.s (100 cps) can be measured using a Brookfield Viscometer at 2% solids in water at 25 ° C, 60 rpm, rotation # 1. “Average viscosity” of carboxymethyl cellulose as some times used here refers to carboxymethyl cellulose having a range of about 200 to 4,000 mPa.s (200 to 4,000 cps) (eg, when measured using a Brookfield viscometer at 2% solids in water, 25 ° C, at 30 rpm, speed n ° 2). Any carboxymethyl cellulose that has a viscosity greater than "medium viscosity" can be considered "high viscosity" carboxymethyl cellulose (and such viscosity can be measured using a Brookfield Viscosimeter at 2% solids in water, 25 ° C, at 30 rpm, speeds 3 or 4).
    [0011] Additionally, edible food products are disclosed that contain the present compositions. These food products can include aqueous systems, emulsions, beverages, sauces, soups, condiments, dairy products and non-dairy products, frozen desserts, and cultured foods. Edible food products may additionally comprise various edible materials and additives, including proteins, fruit juices, vegetable juices, substances with a fruit flavor, or any combination thereof. In addition, a number of industrial suspensions are disclosed that comprise the present compositions that are adapted for use in pharmaceuticals, cosmetics, veterinary products, personal care products, agricultural products, or chemical formulations.
    [0012] Microcrystalline cellulose
    [0013] Any MCC can be employed in compositions of the present invention. MCC from any source can be employed in the compositions of the present invention. Raw materials from which MCC can be obtained include, for example, wood pulp (such as bleached sulphite and sulphate pulps), corn straw, cane bagasse, straw, cotton, cotton yarn, linen, hemp, ramie, algae cellulose and fermented cellulose. Additional raw materials include bleached softwood kraft pulps, bleached hardwood kraft pulps, bleached Eucalyptus kraft pulps, paper pulps, fluff pulps, dissolving pulps, and bleached non-cellulose pulps. In one embodiment, the MCC used is once approved for human consumption by the United States Food and Drug Administration.
    [0014] Microcrystalline cellulose can be in any suitable form. Microcrystalline cellulose is preferably co-rubbed in the form of a "wet cake". The wet microcrystalline cellulose cake is a microcrystalline cellulose that has been manufactured in a wet form (eg containing water) and has not been dried (“never dry”). In other words, a wet microcrystalline cellulose cake is microcrystalline cellulose that has not been previously dried and rehydrated with water. Microcrystalline Cellulose (MCC) can comprise small stem type microcrystals of partially hydrolyzed cellulose (beta 1,4 glucan). Beta 1,4 glucan can be derived from any desired chemical degradation method applied to a selected cellulose material.
    [0015] Microcrystalline cellulose is produced by treating a cellulose source, preferably alpha cellulose in the form of pulp from fibrous plant materials, with a mineral acid, preferably hydrochloric acid (acid hydrolysis). The acid selectivity attacks the less ordered regions of the cellulose polymer chain thus exposing and leaving free the crystalline sites that form aggregates of crystallites that constitute microcrystalline cellulose. These are then separated from the reaction mixture, and washed to remove degraded by-products. The resulting wet mass, generally containing 40 to 60 percent moisture, is referred to in the art by several names, including "hydrolyzed cellulose", "hydrolyzed cellulose cake", "DP cellulose out of level", "wet cellulose cake" microcrystalline ”, or simply“ moist pie ”.
    [0016] The classic process for producing MCC is acid hydrolysis of purified cellulose, first performed by O. A. Battista (U.S. Pat. 2978446, 3023104, and 3146168). Various chemicals or mechanical treatments can be used to enhance MCC acid hydrolysis. In efforts to reduce cost while maintaining or improving the quality of MCC, several alternative processes have also been proposed. These include steam blast (US Pat. 5769934, Hanna et. Al), reactive extrusion (US Pat. 6228213, Hanna et al), one-step hydrolysis and bleaching (World Patent Publication W001 / 0244, Schaible et al) , and partial hydrolysis of a semicrystalline cellulose and water reaction liquor in a reactor pressurized with oxygen and / or carbon dioxide gas and operating at 100 ° C to 200 ° C (US Pat. 5,543,511).
    [0017] Carboxymethyl Cellulose
    [0018] The carboxymethyl cellulose used in the present invention in component (ii) is very specific and has a degree of substitution from 0.95 to 1.5 and a viscosity of less than 100 mPa.s (100 cps). Such a carboxymethyl cellulose is considered in the field to have a high degree of substitution and a very low viscosity (and, as such, it is sometimes referred to here as "high DS / low viscosity CMC"). In more particular modalities, the degree of substitution can be 1.0 - 1.5, more specifically, 1.0 - 1.4, and 1.1 - 1.3, and the viscosity can be from 2 to 100 mPa .s (100 cps), more specifically, from 2 to 50 mPa.s (2 to 50 cps), from 2 to 35 mPa.s (2 to 35 cps), from 2 to 30 mPa.s (2 to 30 cps ), and 2 to 25 mPa.s (2 to 25 cps).
    [0019] Such a carboxymethyl cellulose may be an alkyl metal carboxymethyl cellulose, more particularly sodium, potassium, or ammonium carboxymethyl cellulose, and more preferably sodium carboxymethyl cellulose.
    [0020] Carboxymethyl cellulose is characterized by, among other things, the degree of substitution (sometimes referred to here as "DS"). The DS represents the average number of hydroxyl groups replaced per anhydroglucose unit. For example, each anhydrous glucose unit in carboxymethyl cellulose contains three hydroxyl groups, which give carboxymethyl cellulose a theoretical maximum DS of 3.0.
    [0021] Commercially available carboxymethyl cellulose having a DS of 0.95 - 1.5 is Ambergum 1221 (Ashland, a low viscosity carboxymethyl cellulose having a DS of about 1.2).
    [0022] Preferably, the co-rubbed stabilizing composition of the present invention further comprises component (iii) at least one of a carboxymethyl cellulose having a degree of substitution of less than 0.45 to 0.9 or a carboxymethyl cellulose having a DS of 0.95 to 1.5 and a viscosity of 200 - 4,000 mPa.s (200 - 4,000 cps). Such carboxymethyl celluloses also include the alkyl metal salts thereof such as sodium, potassium or ammonium carboxymethyl cellulose. The carboxymethyl cellulose of component (iii) can have an average viscosity of 200 to 4,000 mPa.s (200 cps to 4,000 cps), preferably 200 mPa.s to 1000 mPa.s (200 cps to 1000 cps), with DS between 0 , 45 to about 0.9. A particular example of this medium low-viscosity DS CMC is Aquaion 7MF series from Ashland. The carboxymethyl cellulose of component (iii) can also have a low viscosity of 5 mPa.s to 200 mPa.s (5 cps to 200 cps), preferably 5 mPa.s to 100 mPa.s (5 cps to 100 cps), with DS between 0.45 to about 0.9. A particular example of this low-viscosity DS CMC is Aquaion 7LF from Ashland. In addition, the carboxymethyl cellulose of component (iii) can also have a viscosity of 200 to 4000 mPa.s (200 cps to 4000 cps), preferably 200 mPa.s to 1000 mPa.s (200 cps to 1000 cps), with DS between about 0.95 to about 1.5. Particular examples of such high DS-medium viscosity CMCs include Aquaion 12M8F and 12M31P, all from Ashland.
    [0023] Generally, microcrystalline cellulose is present in an amount of about 60 - 96%, more preferably 80-95%, more preferably 80- 90%, all based on the total weight of the component's microcrystalline cellulose and carboxymethyl cellulose (ii), and the carboxymethyl cellulose of component (ii) is present in an amount of 4-40%, more preferably 5-20%, more preferably, 10-20%, all based on the total weight of the microcrystalline cellulose and carboxymethyl cellulose of component (ii). In addition, if the carboxymethyl cellulose of component (iii) is present, then the carboxymethyl cellulose of component (iii) may be present in an amount of 2-36%, more preferably, 2-20%, more preferably, 2-15% , all based on the total weight of the stabilizer composition.
    [0024] The stabilizer compositions may consist only of MCC in component (i) and the carboxymethyl cellulose of component (ii). Also, the stabilizer compositions can consist only of the MCC in the component (i), the carboxymethyl cellulose of the component (ii) and the carboxymethyl cellulose of the component (iii). The co-rubbed stabilizing composition of the present invention may contain less than 5% starch, less than 4% starch, less than 3% starch, less than 2% starch, less than 1% starch, all based on total weight of the stabilizer or contain no starch. In addition, the stabilizing composition of the present invention may or may not include any friction aid such as a salt.
    [0025] Historically, when attempts were made to make colloidal MCC with high DS (e.g., 0.9-1.5) / medium viscosity (200-4000 cps), the friction between MCC and CMC would be very slippery, unable to generate adequate work profile. Tests have also shown unsatisfactory performance in food applications. It has been discovered by the present inventors that if low-viscosity DS CMC is used in the MCC / CMC friction / extrusion, the behavior has changed significantly as opposed to using medium or high DS-viscosity CMC. The colloidal MCC / CMC resulting from the present invention performed excellently in food applications, such as soy drinks.
    [0026] More synergy in friction / extrusion was discovered with the addition of a second CMC, which contributes to the remarkable food performance as well.
    [0027] Co-friction
    The present invention is also directed to a method for making the stabilizing composition of the present invention, comprising: a) mixing microcrystalline cellulose and carboxymethyl cellulose of component (ii); b) co-rubbing the mixture from step a); and c) drying the extrudate from step b). The carboxymethyl cellulose of component (iii), if present, is added in step a). As used here, the terms "co-rubbed", "rubbed" and "rubbed" are used interchangeably to mean a process that effectively reduces the size of at least some if not all particles to a colloidal size. “Co-friction” is a term used to refer to the application of shear forces to a mixture of components. Suitable friction processes can be accompanied, for example, by co-extruding, grinding, mixing, or kneading. MCC is typically wet cake having a solids level of between 35 - 70, but can be used in dry or rehydrated form. In addition to various types of extrudates as practiced in the manufacture of current MCC, other examples of wet cake attrition equipment or MCC: CMC include rollers / compression belts, registration rollers, mechanical refining discs, ultrasonic refines, high pressure homogenizers (including micro fluidic devices), high compression plantar mixtures, and shock / cavitation wave devices. Drying can be accomplished by a variety of means, such as spray drying, oven drying, freeze drying, drum drying, flash drying, fluid bed, vacuum drying, mass drying, or thermal reactor drying. . Drying removes water from the composition to obtain a product that will be recognized by one skilled in the art as a “dry” product. For spray drying, the extrudate is dispersed in water to form a paste, optionally homogenized, and then spray dried. Dried particles formed from spray drying can be reconstituted in a desired aqueous medium or solution to form the compositions, edible food products, and suspensions for industrial application described herein.
    [0029] Formulations Using the Stabilizing Composition
    [0030] The co-rubbed stabilizer compositions of the present invention can act as stabilizers in a variety of industrial and consumer uses. In particular, these applications include food (eg, drink), pharmaceutical, health care, agrochemistry and other industrial applications.
    [0031] The stabilizer compositions, after drying to a powder, can be mixed with an aqueous solution to form a stable colloidal suspension. Edible food products formed using the stabilizer compositions described here are capable of providing stable colloidal properties for extended periods even under acidic pH conditions.
    [0032] Some examples of edible food products include the following: suspensions, sauces (especially low pH / high salt types), reconstituted soups, condiments (including both spoon and pouring condiments), drinks (including those that are treated with heat, for example, by pasteurization or ultra pasteurization, or heat treated using high temperature (UHT) or short high temperature (HTST) or reconstitution processes, UHT processed protein and reconstitution and nutritional drinks, protein drinks low pH processed by UHT, calcium fortified drinks by UHT, milk based drinks by UHT), creams processed by reconstitution and by UHT, low pH frozen desserts (eg, fruit ice cream), systems aerated food, cultured products, dairy-based and non-dairy products (cream, yogurt), and confectionery or cream fillings. More specific examples of beverages containing the stabilizing composition of the invention include dairy beverages, eg dairy beverages containing milk (including low-fat or low-fat milk) and flavored milks such as chocolate milk and strawberry milk, as well as containing milk proteins. plant such as soy protein and walnut protein.
    [0033] The levels of use of stabilizer compositions in food products can vary from about 0.05% to about 3.5% by weight of the total food product, and in some instances it can be from 0.2% to 2% by weight of the total food product.
    [0034] Food products may also include other edible ingredients such as, for example, vegetable or fruit pulps, mineral salts, protein sources, fruit juices, acidulants, sweeteners, buffering agents, pH modifiers, stabilizing salts, or a combination of them. Those skilled in the art will recognize that any number of other edible components can also be added, for example, additional flavorings, dyes, preservatives, pH buffers, nutritional supplements, process aids, and the like. The additional edible ingredients can be soluble or insoluble, and, if insoluble, can be suspended in the food product.
    [0035] Some of the edible food products that may contain the stabilizing composition of the invention may comprise protein and / or fruit juice (e.g., fruit juices containing solids (such as pulp) and nectars are readily stabilized by adding the stabilizing compositions ). In such mixtures having only juice or protein only, the composition of the stabilizer composition and the amount of the stabilizer composition used in the beverage mixture may need to be adjusted accordingly to maintain the desired stability results. Such routine adjustment of the composition is entirely within the capabilities of a person skilled in the art and is within the scope and intention of the present invention. These edible food products can be dry mix products (instant sauces, sauces, soups, instant cocoa drinks, etc.), low pH milk systems (cream / yogurt, yogurt drinks, stabilized frozen yogurt, etc.), foods cooked, and a pasta agent in non-aqueous food systems and low humidity food systems.
    [0036] Suitable juices incorporating the stabilizer composition include fruit juices (including but not limited to lemon juice, lime juice, and orange juice, including variations such as lemonade, lime, or orange, white and red grape juices, pomelo juice, apple juice, pear juice, cranberry juice, blueberry juice, raspberry juice, cherry juice, pineapple juice, pomegranate juice, mango juice, apricot juice or nectar, strawberry juice, kiwi juice) and vegetable juices (including but not limited to tomato juice, carrot juice, celery juice, beet juice, parsley juice, spinach juice, and lettuce juice). Juices can be in any form, including liquid, solid, or semi-solid forms such as gels or other concentrates, ice or ice cream, or powders, and can also contain suspended solids.
    [0037] In another modality, substances with a fruit flavor or other sweeteners, including natural flavors, artificial flavors, or those with other natural flavors ("WONF"), can be used instead of fruit juice. Such fruit-flavored substances may also be in the form of liquids, solids, or semi-solids, such as powders, gels or other concentrates, ices, or ice cream, and may also contain suspended solids.
    [0038] Proteins suitable for edible food products incorporating stabilizing compositions include food proteins and amino acids, which can be beneficial to mammals, birds, reptiles, and fish. Food proteins include animal or vegetable proteins and fractions or derivatives thereof. Animal-derived proteins include milk and milk-derived products such as sour cream, cream, whole milk, low-fat milk, skimmed milk, fortified milk including protein-fortified milk, processed milk and milk products including skimmed milk or milk unsweetened or sweetened whole, overheated and / or condensed, dry milk powders including whole milk powder and dry fat-free milk (NFDM), casein and caseinates, buttermilk and products derived from buttermilk such as milk concentrate buttermilk, buttermilk without lactose, buttermilk without mineral, isolated from buttermilk protein. Egg proteins and egg derivatives can also be used. Plant-derived proteins include walnut and walnut-derived proteins, sorghum, vegetables and vegetable-derived proteins such as soy and soy derived products such as fresh untreated soy, fluid soy, soy concentrate, soy isolate, soy flour , and rice proteins, and all forms and fractions thereof. Food proteins can be used in any available form, including liquid, condensate, or powder. When using a powdered protein source, however, it may be desirable to pre-hydrate the protein source before mixing with stabilizer and juice compositions for added stability of the resulting beverage. When protein is added together with a fruit or vegetable juice, the amount used will depend on the desired end result. Typical amounts of protein range from about 1 to about 20 grams per 8 oz (226.8g) serving the resulting stable edible food products, such as drinks, but may be larger depending on the application.
    [0039] Other products and applications for which the present composition, or stabilizer compositions, can be used include industrial suspensions. In some embodiments, industrial suspensions include compositions present that are adapted for use in pharmaceuticals, cosmetics, personal care products, agricultural products, or chemical formulations. Some application examples include use as an excipient for oral dosage forms such as chewable tablets and tablets, flavor mask for medicated assets (such as APAP, aspirin, ibuprofen, etc.); suspending agent; controlled release agent in pharmaceutical applications; delivery system for flavoring agents and nutraceutical ingredients in food, pharmaceutical, and agricultural applications; direct compression sustained release agent, which can be used in pharmaceutical dosage forms such as tablets, films, and thickeners, suspensions, which can be used in foams, creams, and lotions for personal care applications; suspending agent, which can be used with pigments and fillings in ceramics, dyes, cosmetics, and oral care; ceramic material; delivery system for pesticides including insecticides and other agricultural products.
    [0040] As controls used in the examples below, commercially available co-rubbed MCC and high DS-medium viscosity CMC (with or without a second CMC) were tested in the examples below, under the identical extrusion conditions of the present invention. All commercial control samples failed chocolate food tests. As shown by the examples below, there are commercial colloidal MCC products comprising other high DS CMCs (but with higher viscosities) compared to the present invention in food application performance.
    [0041] Additionally, as shown in the examples below, as the CMC viscosity goes beyond 200 mPa.s (200 cps) in the high DS-medium viscosity range, as shown by the controls (Examples 15-16), samples taken under control friction / extrusion conditions they immediately failed the food tests.
    [0042] If desired, dry colloidal MCC / CMC powders (such as Avicel® CL611 or Avicel® RC591) can be added to the high and rubbed / extruded MCC / CMC DS mixture together to generate food functioning products as shown in a from the examples below. An additional strategy to aid friction may include co-attrition / co-extrusion with direct cooling by adding dry ice (frozen CO2), liquid nitrogen, liquid ammonia, etc. Another approach includes adding / dissolving ammonium salts to the high DS MCC / CMC mixture, which will cool the mixture (especially during friction or extrusion), as well as making the extrudate easier to rub or extrude. Ammonium salts can also depress the dispersion viscosity, facilitating drying of larger solids in spray drying. If mass dried, the colloidal MCC product will be softer and more porous (due to the decomposition / blowing of ammonium salts). Finally, there is an added benefit that the ammonium salts will blow and leave no residual salt in the final product. Ammonium salts can include any water-soluble inorganic salts, such as, but not limited to, ammonium carbonate, ammonium bicarbonate, ammonium chloride, ammonium sulfates, and ammonium phosphates, etc. Ammonium salts can also include any water-soluble organic salts, but not limited to, ammonium acetate, ammonium citrate, ammonium lactate, ammonium formate, ammonium tartrate, ammonium oxalate, and ammonium ascorbate, etc. Ammonium bicarbonate and ammonium carbonate are the preferred salts.
    [0043] Other characteristics and advantages of the modalities that follow will be apparent from the following detailed description and from the claims. The disclosed modalities are exemplary and explanatory only and will not be considered to be restrictive to the invention. Unless otherwise indicated here, all parts, percentages, fractions and the like are by weight. EXAMPLES
    [0044] Brookfield viscosities of the co-rubbed compositions tested below were obtained using an RVT viscometer with an appropriate spindle (typically between 1-4) at 20 rpm and 20 ° to 23 ° C. Viscosities were measured to determine an initial viscosity and an adjusted viscosity after 24 hours.
    [0045] "Gel strength (G ')" refers to the system's reversible stored energy (the elastic module G') and relative to the compositions here is a function of the cellulose concentration. The measurements in the examples were made using a TA instrument rheometer (ARES-RFS3) with oscillatory voltage sweep at 1 Hz and 20 ° C, with a space size of 1.8 mm in a dispersion in water with 2.6 % solids (deionized) after 24 hours.
    [0046] Examples 1-7 (MCC / CMC high DS with low Viscosities <25 mPa.s (25cps), Ambergum 1221)
    [0047] Example 1: Rubbed MCC with high DS-low viscosity CMC
    [0048] MCC wet cake was obtained by acid hydrolysis. She was dehydrated to a solids level of 41.6%. In a Hobart mixer, the MCC wet cake was mixed with CMC Ambergum 1221 (Ashland, Inc., Wilmington, DE, USA) in a fraction of 85.15 parts by weight for several minutes. The mixture was passed through a twin screw co-rotation extruder several times with sufficient working profile. The MCC: CMC extrudate was then dispersed in deionized water. The resulting slurry was passed through a Manton Gaulin homogenizer at 17.23 MPa at 20, 68 MPa (2500 to 3000 psi) and spray dried in a 3 foot (91.44 cm) spray dryer to form a powder . When the dry MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 520 mPa.s (520 cps) and an adjusted viscosity after 24 hours of 1,030 at room temperature. mPa.s (1,030 cps).
    [0049] Example 2: MCC rubbed with high DS-Low viscosity CMC (Ambergum 1221)
    [0050] This test was generally conducted as in Example 1, except that the MCC: CMC fraction was 80%: 20% and the solids level of the MCC wet cake was redispersed in deionized water at 2.6% solids , he exhibited an initial Brookfield viscosity of 280 mPa.s (280 cps) and a viscosity adjusted after 24 hours of 680 mPa.s (680 cps) at room temperature. The dispersion of 2.6% solids was measured after 24 hours and exhibited a gel strength of 18 Pa. A colloidal content of 64.2% was obtained.
    [0051] Example 3: MCC Co-rubbed with High DS-Low Viscosity CMC (Ambergum 1221) and Low DS-Low Viscosity CMC (7LF)
    [0052] MCC was co-rubbed with two types of CMCs: Ambergum 1221 (CMC high DS, low viscosity) and CMC Aquaion 7LF (CMC low DS, low viscosity). The MCC: CMC fraction was 80% MCC: 14% Ambergum 1221: 6% Aquaion 7LF CMC. MCC wet cake was obtained by acid hydrolysis. She was dehydrated to a solids level of 41.6%. In a Hobart mixer, the MCC tumble was mixed with CMC Ambergum 1221 (Ashland, Inc., Wilmington, DE, USA) as well as CMC Aquaion 7LF in a fraction of 80: 14: 6 parts by weight for several minutes. The mixture was passed through a twin screw co-rotation extruder several times with sufficient working profile. The MCC: CMC extrudate was then dispersed in deionized water. The resulting slurry was then spray dried in a 3 foot (91.44 cm) dryer to form a powder. When the spray dried MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 1000 mPa.s (1000 cps) and an adjusted viscosity after 24 hours at room temperature. 3,000 mPa.s (3,000 cps). The dispersion of 2.6% solids was measured after 24 hours and exhibited a G 'gel strength of 50 Pa. A colloidal content of 85.7% was obtained.
    [0053] Example 4: MCC co-rubbed with CMC of high DS-low viscosity (Ambergum 1221) and CMC of low DS- low viscosity (7LF)
    [0054] This test was conducted as in Example 3, except the MCC: CMC fraction was 84% MCC: 12% Ambergum 1221: 4% CMC Aquaion 7LF. When the dry MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 1000 mPa.s (1000 cps) and an adjusted viscosity after 24 hours of 2600 at room temperature. mPa.s (2600 cps).
    [0055] Example 5: MCC Co-rubbed with CMC of high DS-low viscosity (Ambergum 1221) and CMC of low DS-Medium viscosity (7MF)
    [0056] This test was conducted as in Example 3, except that the MCC: CMC fraction was 80% MCC: 14% Ambergum 1221: 6% CMC Aquaion 7MF. When the dry MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 3400 mPa.s (3400 cps) and an adjusted viscosity after 24 hours of 3600 at room temperature. mPa.s (3600 cps). The dispersion of 2.6% solids was measured after 24 hours and exhibited a G 'gel strength of 100 Pa. A colloidal content of 91.1% was obtained.
    [0057] Example 6: MCC co-rubbed with CMC of high DS-low viscosity (Ambergum 1221) and CMC of low DS - Medium viscosity (7MF)
    [0058] This test was performed as in Example 3, except that the fraction of MCC: CMC was 80% MCC: 15% Ambergum 1221: 5% CMC Aquaion 7MF. When the dry MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 2425 mPa.s (2425 cps) and an adjusted viscosity after 24 hours of 4000 at room temperature. mPa.s (4000 cps).
    [0059] Example 7: MCC co-rubbed with high DS-low viscosity CMC (Ambergum 1221) and low DS-medium viscosity CMC (7MF)
    [0060] MCC was co-rubbed with two types of CMCs: Ambergum 1221 (CMC high DS, low viscosity) and CMC Aquaion 7MF III (CMC low DS, medium viscosity). The fraction of MCC: CMCs was 80 MCC: 15 Ambergum 1221: 5 CMC Aquaion 7MF. MCC wet cake was obtained by acid hydrolysis. It was then mixed and extruded on a pilot scale adjusted from a twin screw co-rotation extruder. The MCC: CMC extrudate was then dispersed in deionized water. The resulting slurry was then spray dried to form a powder. When the spray dried MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 1800 mPa.s (1800 cps) and an adjusted viscosity after 24 hours at room temperature. 3150 mPa.s (3150 cps). The dispersion of 2.6% solids was measured after 24 hours and exhibited a gel strength of 55 Pa.
    [0061] Examples 8-12 (high DS MCC / CMC with low viscosities> 25 mPa.s (25 cps), <100 mPa.s (100 cps))
    [0062] Example 8: MCC rubbed with high DS-low viscosity CMC (Aquaion 12LF # 17)
    [0063] The high DS, low viscosity CMC used in this example had a viscosity of 38 mPa.s (38 cps) and DS 1.28 (Aquaion 12LF # 17). This test was performed as in Example 2, except that the MCC: CMC fraction was 80% MCC: 20% CMC Aquaion 712LF. When the spray dried MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 800 mPa.s (800 cps) and an adjusted viscosity after 24 hours at room temperature. 850 mPa.s (850 cps). A colloidal content of 37% was obtained.
    [0064] Example 9: MCC co-rubbed with high DS-low viscosity CMC (Aquaion 12LF # 17) and low DS-low viscosity CMC (7LF)
    [0065] MCC was co-rubbed with two types of CMCs: Aquaion 12LF # 17 (1.28 DS, viscosity 38 mPa.s (38 cps)) and CMC Aquaion 7LF (a low DS CMC, low viscosity). The fraction of MCC: CMC was 80% (MCC): 14% (Aquaion 12LF # 17): 6% (CM Aquaion 7LF). MCC wet cake was obtained by cooking by acid hydrolysis. She was dehydrated to a solids level of 41.6%. In a Hobart mixer, the MCC wet cake was mixed with CMC Aqualon 12LF # 17 (Ashland, Inc., Wilmington, DE, USA) as well as CMC Aqualon 7LF in a fraction of 80: 14: 6 parts by weight for several minutes. The mixture was passed through a twin screw co-rotation extruder several times with sufficient working profile. The MCC: CMC extrudate was then dispersed in deionized water. The resulting slurry was then spray dried in a 3 foot (91.44 cm) Bowen spray dryer to form a powder. When the spray-dried MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 600 mPa.s (600 cps) and an adjusted viscosity after 24 hours of 2050 mPa.s (2050 cps). A colloidal content of 61.5% was obtained.
    [0066] Example 10: MCC Co-rubbed with CMC of high DS-low viscosity (Aqualon 12LF # 24 and CMC of low DS-low viscosity (7LF)
    [0067] MCC was co-rubbed with two types of CMCs: Aqualon 12LF # 24 (1.30 DS, viscosity 36 mPa.s (36 cps)) and CMC Aqualon 7LF (a low DS CMC, low viscosity). The MCC: CMC fraction was 80% (MCC): 14% (Aqualon 12LF # 24): 6% (CM Aqualon 7LF). MCC wet cake was obtained by acid hydrolysis.
    [0068] She was dehydrated at a solids level of 41.6%. In a Hobart mixer, the MCC wet cake was mixed with CMC Aqualon 12LF # 24 (Ashland, Inc., Wilmington, DE, USA) as well as CMC Aqualon 7LF in a fraction of 80: 14: 6 parts by weight for several minutes. The mixture was passed through a twin screw co-rotation extruder several times with sufficient working profile. The MCC: CMC extrudate was then dispersed in deionized water. The resulting slurry was then spray dried in a 3 foot (91.44 cm) Bowen spray dryer to form a powder. When the spray dried MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 275 mPa.s (275 cps) and an adjusted viscosity after 24 hours. 1600 mPa.s (1600 cps). A colloidal content of 55.7% was obtained.
    [0069] Example 11: MCC rubbed with another type of high DS low viscosity CMC (Aqualon 12LF # 24)
    [0070] This example was performed in the same way as Example 2, except that the fraction of MCC: CMC was 85% MCC: 15% CMC Aqualon 12LF # 24 and during extrusion, dry ice (30% by weight) of dry weight extrudate) was added to cool the extrudate directly. When the spray dried MCC: CMC powder was dispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 1000 mPa.s (1000 cps) and an adjusted viscosity after 24 hours of 1125 mPa.s (1125 cps).
    [0071] Example 12: High DS-low viscosity CMC (Aqualon 12FL # 24)
    [0072] MCC was co-rubbed with Aqualon 12LF # 24 (1.30 DS, viscosity 36 mPa.s (36 cps)) and dry powder of Avicel® RC-591. The use of dry powder Avicel® RC-591 intensified the intensity of extrusion. MCC wet cake was obtained by acid hydrolysis. He was dehydrated at a solids level of 41.6%. In a Hobart mixer, the MCC wet cake was mixed with CMC Aqualon 12LF # 24 (Ashland, Inc., Wilmington, DE, USA) as well as Avicel® RC-591 in a fraction of 64:16:20 parts by weight , respectively, for several minutes. The mixture was passed through a twin screw co-rotation extruder several times with sufficient working profile. The resulting extrudate was then dispersed in deionized water. The resulting slurry was then spray dried in a 3 foot (91.44 cm) Bowen spray dryer to form a powder. When the spray dried powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 2750 mPa.s (2750 cps) and an adjusted viscosity after 24 hours of 2600 mPa.s at room temperature. (2600 cps). A colloidal content of 86.9% was obtained.
    [0073] Example 13: MCC Co-rubbed with CMC of high DS-low viscosity (Ambergum 1221) and CMC of high DS-medium viscosity (12M8F)
    [0074] This test was performed in the same way as in Example 3, except that the fraction of MCC: CMC was 80% MCC: 14% Ambergum 1221: 6% CMC Aquaion 12M8F. When the dry MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 1000 mPa.s (1000 cps) and an adjusted viscosity after 24 hours of 1500 mPa at room temperature. .s (1500 cps). A colloidal content of 64.9% was obtained.
    [0075] Comparative Examples (14-17)
    [0076] Example 14: MCC rubbed with high DS CMC, medium viscosity (12M8F) under Control Conditions
    [0077] MCC wet cake was obtained by acid hydrolysis. She was dehydrated to a solids level of 41.6%. In a Hobart mixer, the wet MCC cake was mixed with CMC Aquaion 12M8F (Ashland, Inc., Wilminton, DE, USA) in a fraction of 80:20 parts by weight for several minutes. The mixture was passed through a twin screw co-rotation extruder several times. The MCC: CMC extrudate was then dispersed in deionized water. The resulting slurry was then spray dried in a 3 foot (91.44 cm) spray dryer. When the spray dried MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 740 mPa.s (740 cps) and an adjusted viscosity after 24 hours of 1800 mPa.s (1800 cps). Food tests on chocolate milk failed immediately, due to heavy sedimentation.
    [0078] Example 15: MCC co-rubbed with CMC of high DS-Medium viscosity (12M8F) and CMC of low DS, under Control Conditions
    [0079] The experiment was carried out in a manner similar to that of Example 14, except that two types of CMC were used during co-friction / extrusion. The fraction was 80% MCC: 10% 12M8F: 10% CMC 7LF. When the spray-dried MCC: CMC powder was redispersed in deionized water at 2.6% solids, it exhibited an initial Brookfield viscosity of 67 mPa.s (67 cps) and an adjusted viscosity after 24 hours. 1260 mPa.s (1260 cps). Food testing in chocolate milk failed immediately, due to heavy sedimentation and phase separation.
    [0080] Example 16: Commercial Colloidal MCC Comprising High DS CMC, Medium Viscosity and Salt
    [0081] A commercially available colloidal MCC comprising high DS CMC, medium viscosity and salt (as a friction aid) was dispersed in 2.6% solids deionized water. He exhibited an initial Brookfield viscosity of 1650 mPa.s (1650 cps) and an adjusted viscosity after 24 hours of 3250 mPa.s (3250 cps) at room temperature. A colloidal content of 80% was obtained, which was determined by centrifuging the water dispersion at 8250 rpm for 5 minutes followed by gravimetric analysis of the dry supernatant portion. This commercially available stabilizer is considered to be among the best performers and is used here as a reference to compare the performance of the stabilizers of the present invention (using a different CMC and without friction aid).
    [0082] Example 17: Commercial Colloidal MCC Comprising Low DS CMC (eg Avicel® RC-591)
    [0083] When dispersed in 1.2% solids deionized water, this sample exhibited an initial Brookfield viscosity of 40-175 mPa.s (40 - 175 cps) and an adjusted viscosity after 24 hours from 800 to 1600 mPa.s (800 to 1600 cps).
    [0084] Examples 18-21: Food Applications
    [0085] Example 18: Chocolate milk drinks by UHT
    [0086] Materials and Methods:
    [0087] UHT chocolate drink samples were prepared using: A) Commercial colloidal MCC / high DS CMC, medium viscosity as described in Example 16 (control sample); B) colloidal MCC / CMC of high DS-low viscosity as in Example 2 (inventive sample); C) colloidal MCC / CMC of high DS-low viscosity and CMC of low DS-low viscosity as in Example 3 (inventive sample); D) colloidal MCC / mixture of high DS-low viscosity CMC and low DS-low viscosity CMC as in Example 4 (inventive sample); E) Colloidal MCC / mixture of high DS-low viscosity CMC and high DS-medium viscosity CMC as in Example 13 (inventive sample). The formulations are shown in Table 1.
    [0088] Table 1

    [0089] Process:
    [0090] All powders were mixed together dry and mixed for 30 minutes with the milk using a simple elevated mixing apparatus (Lightnin Mixer). each sample was processed using a Micro Thermics® UHT / HTST Direct & Indirect Processing System assembled to deliver the following temperature and retention time sequences. The unprocessed mixture was first preheated to 185 ° F (85 ° C) followed by immediate indirect steam sterilization in the final heater. The resulting product was kept at 284 ° F (140 ° C) for 6 seconds followed by cooling to 150 ° F (65.5 ° C). Two-stage homogenization was employed (17.23 MPa (2,500 cps) first stage / 3.44 MPa (500 psi) second stage). The sterile mixture was further cooled to ~ 70 ° F (21.1 ° C) where the product was filled into clean% liter liter nalgen bottles within a clean Sterile Product Outlet & Protection. One set of bottles was placed in cold storage at 40 ° F (4.44 ° C) and the second set was placed on a shelf at room temperature (70 ° F (21.1 ° C)). Drinks were analyzed for viscosity, pH, and physical stability at 1 day, 1 week, 2 weeks, 1 month, and 3 months of shelf life. Each test period consisted of the following observations.
    [0091] Table 2: Visual Parameters


    [0092] Table 3: One Month of Observation

    [0093] Viscosity determined using a Brookfield LVF Viscometer at 60 rpm, rotation # 1 at 70 ° F (21.1 ° C)
    [0094] # Viscosity determined using a Brookfield LVF Viscometer at 60 rpm, rotation # 1 at 40 ° F (4.44 ° C)
    [0095] Conclusion (one month observation): Visual defects associated with instability in chocolate drinks are generally seen within the first few hours after filling the containers. In UHT chocolate milk applications stabilized with colloidal microcrystalline cellulose, the most prominent sign of instability is the sedimentation of the cocoa particles. Commercial sample A used as a control and reference consistently provided excellent suspension of cocoa particles with minimal viscosity and no sign of gelling. Inventive samples B, C, D and E were unexpectedly found to provide equivalent stability characteristics such as Control Sample A revealing no sign of sedimentation and no visual sign of gelling. Among these samples in the case of refrigerated conditions, Sample B showed some mild marbling, but was still effective. Samples C, D, and E had ideal stabilization. These results indicate that the stabilizer of the present invention provided an unexpected level of stabilization and was comparable to a commercial high performance product. The additional tests that were performed as shown in Table 2 showed no defects for samples A-E.
    [0096] Example 19: UHT Chocolate Milk Drinks
    [0097] Materials and Methods:
    [0098] Samples of UHT chocolate drinks were prepared using A) commercial colloidal MCC / high DS CMC, medium viscosity as described in Example 16 (control sample); B) Colloidal MCC / CMC of high DS-low viscosity and CMC of low DS-medium viscosity as in Example 6 (inventive sample); C) Colloidal MCC done on a pilot scale / mixture of CMC of high DS-low viscosity and CMC of low DS-medium viscosity as in Example 7 (inventive sample). The formulations are shown in Table 4.
    [0099] Table 4

    [00100] Process:
    [00101] All powders were mixed together dry and mixed for 30 minutes with the milk using a simple elevated mixing apparatus (Lightnin Mixer). Each sample was processed using a Micro Thermics® UHT / HTST Direct & Indirect Processing System assembled to deliver the following temperature and retention time sequences.
    [00102] The unprocessed mixture was first preheated to 185 ° F (85 ° C) followed by immediate indirect steam sterilization in the final heater. The resulting product was kept at 284 ° F (140 ° C) for 6 seconds followed by cooling to 150 ° F (65.5 ° C). Two-stage homogenization was employed (17.23 MPa (2,500 cps) first stage Z3.44 MPa (500 psi) second stage). The sterile mixture was further cooled to ~ 70 ° F (21.1 ° C) where the product was filled into clean% liter liter nalgen bottles within a clean Sterile Product Outlet & Protection. One set of bottles was placed in cold storage at 40 ° F (4.44 ° C) and the second set was placed on a shelf at room temperature (70 ° F (21.1 ° C)). Drinks were analyzed for viscosity, pH, and physical stability.
    [00103] Visual parameters and scale, are described in Table 2.
    [00104] Table 5: An Observation Week

    [00105] Viscosity determined using a Brookfield LVF Viscometer at 60 rpm, rotation # 1 at 70 ° F (21.1 ° C)
    [00106] # Viscosity determined using a Brookfield LVF Viscometer at 60 rpm, rotation # 1 at 40 ° F (4.44 ° C)
    [00107] Conclusion (one week observation): Sample A provided good stability with no sign of gelling and very little sedimentation of some cocoa particles. Samples B and C were found to provide excellent stability with no sign of sedimentation and no visual sign of gelation. The additional tests that were performed as shown in Table 2 did not show any defects for samples A-C. As a result, the stabilizers of the present invention tested in this Example were unexpectedly found to be superior to the high performance commercial product.
    [00108] Example 20: UHT Soy Drink
    [00109] Materials and Methods:
    [00110] UHT soy beverage samples were prepared using A) commercial colloidal MCC / high DS CMC, medium viscosity as described in Example 16 (control sample); B) colloidal MCC / CMC of high DS-low viscosity as in Example 2 (inventive sample); C) Colloidal MCC / mixture of high DS-low viscosity CMC and low DS-CMC low viscosity as in Example 4 (inventive sample). The formulations are shown in Table 6.
    [00111] Table 6

    [00112] Process:
    [00113] Isolated soy protein, sodium citrate, and 600 g of sugar were added to water heated to 167 ° F (75 ° C). Materials were allowed to hydrate while gently mixing with a Silverson mixer to prevent foam. A dry mix of colloidal MCC stabilizer and 200 grams of sugar were added to the mixture and left to stir for 5 minutes. The remaining sugar and TCP were then added and left to mix for an additional 5 minutes. The pH was checked and recorded. The product was then transferred to the UHT / HTST Micro Thermics® Direct & Indirect Processing System assembled to deliver the following temperature and retention time sequences. The unprocessed mixture was first preheated to 176 ° F (80 ° C) followed by immediate indirect steam sterilization in the final heater. Product was kept at 284 ° F (140 ° C) for 6 seconds followed by cooling to 150 ° F (65.5 ° C). Two-stage homogenization was employed (17.23 MPa (2,500 cps) first stage / 3.44 MPa (500 psi) second stage). The sterile mixture was further cooled to ~ 70 ° F (21.1 ° C) where the product was filled into clean% liter nalgen bottles inside a Sterile Product Outlet & clean filling protection. Bottles were stored at 4 ° C, 20 ° C and 30 ° C. Drinks were analyzed for stability based on visual parameters and scale as described previously in Table 2 (Example 20).
    [00114] Conclusion (two weeks of observation): Samples B, C, and D provided good functionality and very little sediment (such sediment being very easy to re-disperse) and such results were comparable to Sample A of high commercial performance. The additional tests that were performed as shown in Table 2 did not show defects for samples A-D.
    [00115] Example 21: UHT Soy Drink
    [00116] Materials and Methods:
    [00117] Samples of UHT soy drinks were prepared using A) commercial colloidal MCC / high DS CMC, medium viscosity as described in Example 16 (control sample); B) colloidal MCC / CMC of high DS-low viscosity as in Example 6 (inventive sample); C) Pilot scale colloidal MCC / mixture of high DS-low viscosity CMC and low DS-CM medium viscosity as in Example 7 (inventive sample). The formulations are shown in Table 7.
    [00118] Table 7


    [00119] Process:
    [00120] Isolated soy protein, sodium citrate, and 300 g of sugar were added to the water heated to 75 ° C. Materials were allowed to hydrate while gently mixing with a Silverson mixer to prevent foam. A dry blend of colloidal MCC stabilizer and 40 grams of sugar were added while mixing. The remaining sugar and TCP were then added and allowed to mix. The pH was checked to ensure ~ pH 7. The product was then transferred to the UHT Processing System (SPC Plate Heat Exchanger) assembled to deliver the following temperature and retention time sequences. The unprocessed mixture was first preheated to 80 ° C, followed by homogenization upstream to 200 bar (150 first stage / 50 second stage). The mixture was heated to 140 ° C for 5 seconds followed by cooling to 10 ° C. The sterile product was filled aseptically into clean 250 ml Nalgene bottles. Bottles were stored at 4 ° C. Drinks were analyzed for viscosity, pH and stability based on visual parameters and scale as previously described in Table 2.
    [00121] Conclusion (one day of observation): All samples suspended the calcium perfectly. No defects were observed. Samples B and C showed higher viscosities even at the least significant dosages, indicating an unexpected and better stabilization than the high performance commercial Sample A. The additional tests that were performed as shown in Table 2 showed no defects for samples A-C.
    [00122] While the invention is being described in detail and with reference to its specific modalities, it will be apparent to a person skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the same.
    权利要求:
    Claims (18)
    [0001]
    1. Co-rubbed stabilizing composition, comprising: (i) microcrystalline cellulose and (ii) at least 4% by weight of carboxymethyl cellulose, based on the total weight of components i) -ii); and characterized by the fact that said carboxymethyl cellulose has a substitution degree of 0.95-1.5 and a Brookfield viscosity of less than 100 mPa.s (100 cps) measured using a Brookfield viscometer at 2% solids in water at 25 ° C, at 60 rpm, rotation n ° 1.
    [0002]
    2. Stabilizing composition, according to claim 1, characterized by the fact that said viscosity is less than 50 mPa.s (50 cps).
    [0003]
    3. Stabilizing composition, according to claim 1, characterized by the fact that said viscosity is less than 25 mPa.s (25 cps).
    [0004]
    4. Stabilizing composition according to claim 1, characterized by the fact that microcrystalline cellulose is present in an amount of 60-96% by weight of the microcrystalline cellulose and carboxymethyl cellulose in said stabilizing composition, and said carboxymethyl cellulose is present in an amount of 4 to 40% by weight of the microcrystalline cellulose and carboxymethyl cellulose in said stabilizing composition.
    [0005]
    5. Stabilizer composition according to claim 1, characterized in that it comprises (iii) at least one of a carboxymethyl cellulose having a degree of substitution of less than 0.45 to 0.9 or a carboxymethyl cellulose having a DS 0.95 to 1.5 and a Brookfield viscosity of 200 - 4,000 mPa.s (200 - 4,000 cps) measured using a Brookfield viscometer at 2% solids in water at 25 ° C, 60 rpm, rotation n ° 1.
    [0006]
    6. Stabilizer composition according to claim 5, characterized by the fact that the carboxymethyl cellulose of component (iii) is present in an amount of 2 to 36% by weight of the total stabilizer composition.
    [0007]
    7. Stabilizing composition according to claim 5, characterized by the fact that said component (iii) carboxymethyl cellulose having a DS of between 0.45 to 0.9 has a viscosity of 200 to 4,000 mPa.s (200 to 4,000 cps) or a viscosity of 5 to 200 mPa.s (5 to 200 cps).
    [0008]
    8. Stabilizing composition according to claim 1, characterized by the fact that said carboxymethyl cellulose has a degree of substitution of 1.0 - 1.5.
    [0009]
    9. Stabilizing composition according to claim 5, characterized by the fact that it consists of said microcrystalline cellulose, said carboxymethyl cellulose of component (ii) and said carboxymethyl cellulose of component (iii).
    [0010]
    10. Stabilizer composition according to claim 1, characterized in that said stabilizer does not contain a starch.
    [0011]
    11. Food, characterized by the fact that it comprises the stabilizer composition as defined in claim 1, in which the stabilizer composition is present in an amount of 0.05 to 3.5% of the total weight of the drink.
    [0012]
    12. Food according to claim 11, characterized by the fact that the food is a drink.
    [0013]
    13. Food according to claim 12, characterized by the fact that the drink has a pH of 2-7.
    [0014]
    14. Food according to claim 13, characterized by the fact that the drink comprises at least one of milk protein or plant protein.
    [0015]
    15. Food according to claim 14, characterized by the fact that said plant protein comprises at least one among soy protein or walnut protein.
    [0016]
    16. Industrial composition, characterized by the fact that it comprises the stabilizer as defined in claim 1.
    [0017]
    17. Method for making the stabilizing composition as defined in claim 1, characterized in that it comprises: a) mixing the microcrystalline cellulose and carboxymethyl cellulose of the component (ii) defined in claim 1, b) co-attriting the mixture from step a) , and c) drying the extrudate from step b).
    [0018]
    18. The method of claim 17, characterized by the fact that it comprises mixing the carboxymethyl cellulose of component (iii) of claim 5 in step a).
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    同族专利:
    公开号 | 公开日
    EP2787837B1|2017-03-15|
    CN104010522A|2014-08-27|
    BR112014013792A8|2017-06-13|
    BR112014013695B1|2020-11-10|
    EP2787837A4|2015-05-20|
    WO2013085809A1|2013-06-13|
    BR112014013695A2|2017-06-13|
    ES2628612T3|2017-08-03|
    WO2013085810A2|2013-06-13|
    EP2787837A2|2014-10-15|
    BR112014013695A8|2017-06-13|
    BR112014013792A2|2017-06-13|
    US8927609B2|2015-01-06|
    US20130150462A1|2013-06-13|
    US20140364514A1|2014-12-11|
    EP2787836A1|2014-10-15|
    PL2787837T3|2017-09-29|
    EP2787836A4|2015-05-27|
    BR112014013792B8|2020-11-10|
    CN103987273A|2014-08-13|
    CN103987273B|2018-07-27|
    US9828493B2|2017-11-28|
    WO2013085810A3|2013-08-01|
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    法律状态:
    2018-05-02| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2019-02-05| B25G| Requested change of headquarter approved|Owner name: FMC CORPORATION (US) |
    2019-02-19| B25A| Requested transfer of rights approved|Owner name: DUPONT NUTRITION USA, INC. (US) |
    2019-07-30| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2019-12-24| B15K| Others concerning applications: alteration of classification|Free format text: AS CLASSIFICACOES ANTERIORES ERAM: A23L 1/0534 , C08L 1/02 , C08L 1/28 Ipc: A23L 29/262 (2016.01), C08L 1/02 (1974.07), C08L 1 |
    2019-12-24| B06A| Patent application procedure suspended [chapter 6.1 patent gazette]|
    2020-04-07| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-09-15| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 30/11/2012, OBSERVADAS AS CONDICOES LEGAIS. |
    2020-11-10| B16C| Correction of notification of the grant [chapter 16.3 patent gazette]|Free format text: REF. RPI 2593 DE 15/09/2020 QUANTO AO ENDERECO. |
    优先权:
    申请号 | 申请日 | 专利标题
    US201161568672P| true| 2011-12-09|2011-12-09|
    US61/568,672|2011-12-09|
    PCT/US2012/067244|WO2013085810A2|2011-12-09|2012-11-30|Co-attrited stabilizer composition|
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