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    granulation of a stevia sweetener. A method for preparing a granulated stevia sweetener is described. The resulting sweetener has a desirably high solubility level.
    公开号:BR112012011382B1
    申请号:R112012011382-8
    申请日:2010-11-09
    公开日:2018-02-06
    发明作者:Purkayastha Siddhartha；Markosyan Avetik
    申请人:Purecircle Usa Inc.；
    IPC主号:
    专利说明:

    (54) Title: METHOD TO PRODUCE A SWEETENER AND SWEETENER FROM STEVIA GRANULADO (51) Int.CI .: A23L 1/236 (30) Unionist Priority: 02/04/2010 US 12 / 753.470, 12/11/2009 US 61 /260.465, 12/11/2009 US 61 / 260.593, 03/13/2010 US 12 / 720.888, 12/29/2009 US 61 / 290.778 (73) Owner (s): PURECIRCLE USA INC.
    (72) Inventor (s): SIDDHARTHA PURKAYASTHA; AVETIK MARKOSYAN
    1/16 “METHOD TO PRODUCE A STEVIA GRANULATE SWEETENER AND SWEETENER”
    Field of the Invention
    The invention relates to a process for compacting and granulating individual or combined sweet glycosides of an extract of Stevia rebaudiana Bertoni plant, and more particularly to prepare a substantially powderless granulated sweetener with which Stevia sweeteners may or may not contain co-ingredients such as but not limited to caloric or non-caloric sweeteners, flavor modifiers and taste modifiers.
    Description of the Related Art
    High intensity sweeteners have a level of sweetness often exceeding that of sucrose. They are widely used in the manufacture of reduced calorie or diet food and beverage products. Although a natural caloric sweetener such as sucrose, fructose, and glucose provides consumers with the most desirable taste, they are caloric and cause increases in blood glucose levels. On the other hand, high intensity sweeteners are essentially non-calorie, do not affect the blood glucose level, and provide little or no nutritional value.
    However, high intensity sweeteners that are generally used as sugar substitutes have flavor characteristics that are different than those of sugar, such as sweet taste with different time profile, maximum response, taste profile, mouth feel and / or behavior adaptation. For example, the sweet taste of some high-intensity sweeteners is slower in the beginning and longer in duration than sugar, and thus changes the taste balance of a food composition. Because of these differences, the use of high intensity sweeteners to replace a filler sweetener such as sugar in a food or beverage product causes an imbalance in the time and / or taste profile. If the flavor profile of high intensity sweeteners can be modified to give desired flavor characteristics which are similar, identical, or almost identical to those of sugar or other natural caloric sweeteners, they can provide low calorie drinks and characteristic food products flavor that are most desirable to consumers. To achieve the time profile and / or taste similar to sugar, several ingredients have been suggested.
    On the other hand, high intensity sweeteners can have some cost and functional advantages compared to sugar. Competition between high-sugar and sugar-free sweeteners is strong, for example, in the soft drink industry, especially in countries where their use and production is permitted and similarly in countries with overvalued sugar prices.
    At the moment, high intensity sweeteners are used worldwide. They can be of synthetic and natural origin.
    2/16
    Non-limiting examples of synthetic high-intensity sweeteners include sucralose, acesulfame potassium, aspartame, alitame, saccharin, synthetic neesperidin derivatives dihydrochalcona, cyclamate, neotame, dulcin, suosan, 1-methyl ester of N- [N- [3- ( 3-hydroxy-4-methoxyphenyl) propyl] -La-aspart] -L-phenylalanine, N- [N- [3- (3-hydroxy-4-methoxyphenyl) -3-methilbutyl] -La-aspart] -L -phenylalanine, 1-methyl ester of N- [N- [3- (3-methoxy-4hydroxyphenyl) propyl] -La-aspart] -L-phenylalanine, salts thereof, and the like.
    Non-limiting examples of natural high-intensity sweeteners include Stevioside, Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside E, Rebaudioside F, Steviolbioside, Dulcoside A, Rubusoside, Mogrosides, Brazzein, Dihydrochalcone (NHDC), glycyrrhizal acid and their glycyrrhizal acid thaumatin, perilartine, pernandulcin, mucuroziosides, baiiunoside, flomisoside-l, dimethyl-hexahydrofluorene-dicarboxylic acid, abrusosidos, periandrine, carnosifiosides, cyclocarioside, pterocariosides, polypeptide A, brazilina, dihydrofluorine, glycine, hydrochloride, 3-acetate, neoastilibine, trans-cinnamaldehyde, monatin and its salts, seligueain A, hematoxylin, moneline, osladine, pterocarioside A, pterocarioside B, mabinline, pentadine, miraculin, curculine, neoculin, chlorogenic acid, cinarin, siamenosine and others.
    High intensity sweeteners can be derived from the modification of natural high intensity sweeteners, for example, by fermentation, enzymatic treatment, or derivation.
    At the moment, approximately eleven high-intensity sweeteners are used worldwide. These are acesulfame-K, alitame, aspartame, cyclamate, glycyrrhizin, NHDC, saccharin, Stevioside, sucralose, thaumatin, neotame and Rebaudioside A.
    High intensity sweeteners can be grouped into three generations. The first generation is represented by cyclamate, glycyrrhizin and saccharin, and has a long history of use in food. The second generation includes acesulfame-K, aspartame, NHDC and thaumatin. Alitame, neotame, sucralose, Stevioside, and Rebaudioside A belong to the third generation.
    The standard sweetening power associated with each high intensity sweetener is given in Table 1. However, when they are used in mixtures, the sweetening power can change significantly.
    Table 1
    Sweetness Power of High Intensity Sweeteners
    Sweetener Sweetness power Sucrose 1 Acesulfame-K 200 Alitame 2000 Aspartame 200 Cyclamate 30
    3/16
    Glycyrrhizin 50 NHDC 1000 Saccharin 300 Stevioside 200 Rebaudioside A 450 Thaumatin 3000 Sucralose 600
    On the other hand, 'natural' and 'organic' foods and drinks have become the hottest area in the food industry. The combination of consumer desire, advances in food technology, and new studies linking diet to disease and disease prevention have created an unprecedented opportunity to address public health through diet and lifestyle.
    An increasing number of consumers perceive the ability to control their health by enhancing their current health and / or restricting future illnesses. This creates a demand for food products with increased features and associated health benefits, specifically a trend in the consumer and lifestyle food market for “whole health solutions”. The term natural is highly emotional in the world of sweeteners and has been identified as the one of fundamental trust, along with whole grains, heart healthy and low in sodium. The term 'Natural' is closely related to 'healthier'.
    In this respect, natural high-intensity sweeteners may have better commercial potential.
    Stevia Bertoni rebaudiana is a perennial shrub of the Asteraceae family (Compositae) native to certain regions of South America. The leaves of the plant contain 10 to 20% of diterpene glycosides, which are around 150 to 450 times sweeter than sugar. The leaves have been traditionally used for hundreds of years in Paraguay and Brazil to sweeten local teas and medicines.
    There are currently over 230 species of Stevia with significant sweetening properties. The plant was successful in its development under a wide range of conditions from its subtropic native to the cold northern latitudes.
    Steviol glycosides have zero calories and can be used wherever sugar is used. They are ideal for diabetics and low calorie diets. In addition, sweet steviol glycosides have functional and sensory properties superior to those of many other high intensity sweeteners.
    The Stevia rebaudiana plant extract contains a mixture of different sweet diterpene glycosides, which have a single base - steviol - and differs in the presence of
    4/16 carbohydrate residues in positions C13 and C19. These glycosides accumulate in Stevia leaves and make up approximately 10% - 20% of the total dry weight. Typically, based on dry weight, the four main glycosides found in Stevia leaves are Dulcoside A (0.3%), Rebaudioside C (0.6%), Rebaudioside A (3.8%) and Stevioside (9.1 %). Other glycosides identified in the Stevia extract include Rebaudioside B, C,
    D, E, and F, Steviolbioside and Rubusoside. Among steviol glycosides, only Stevioside and Rebaudioside A are available on a commercial scale.
    The physical and sensory properties are well studied only for Stevioside and Rebaudioside A. The potency of Stevioside sweetness is about 210 times higher than sucrose, Rebaudioside A is between about 200 and about 400 times higher than sucrose , and Rebaudioside C and Dulcoside A are each about 30 times higher than sucrose. Rebaudioside A is considered to have more favorable sensory attributes than the four main steviol glycosides (table 2).
    Table 2
    Physical and Sensory Properties of Steviol Glycosides
    Name Formula TFusion, ° c, WeightMol. Optical rotation [a] 25 D (H 2 O, 1%, w / v) Solubili-water,% Relative sweetness Quality offlavor Steviol C20H30O3 212-213 318.45 ND ND ND Verybitter Steviol-monoside C26H40O8 ND 480.58 ND ND ND ND Stevioside C38H60O18 196-198 804.88 -39.3 0.13 210 Bitter RebaudiosideTHE C44H70O23 242-244 967.01 -20.8 0.80 200-400 Any lessBitter RebaudiosideB C38H60O18 193-195 804.88 -45.4 0.10 150 Bitter RebaudiosideÇ C44H70O22 215-217 951.01 -29.9 0.21 30 Bitter RebaudiosideD C50H80O28 248-249 1129.15 -29.5(ethanol) 1.00 220 similar tosucrose RebaudiosideAND C44H70O23 205-207 967.01 -34.2 1.70 170 similar tosucrose RebaudiosideF C43H68O22 ND 936.99 -25.5(goal-nol) ND Dulcoside A C38H60O17 193-195 788.87 -50.2 0.58 30 Verybitter Steviolbioside C32H50O13 188-192 642.73 -34.5 0.03 90 In-unsavory Rubusosid C32H50O13 ND 642.73 642.73 ND 110 Verybitter
    6/16 cases of granulation or agglomeration are suitable to produce compositions with the desired properties. In particular, it is well known that Rebaudioside A exhibits the so-called polymorphism (Zell et al., Investigation of Polymorphism in Aspartame and Neotame Using Solid-State NMR Spectroscopy. Tetrahedron 56 (6603-6616), 2000) ._ Solvate and anhydrous forms , amorphous Rebaudioside A differ significantly from each other in terms of solubility which is one of the main criteria for the commercial viability of a sweetener. In this respect, as shown in Table 3, the hydrate form of Rebaudioside A exhibits the lowest solubility (Prakash et al., Development of rebiana, a natural, noncaloric sweetener. Food Chem. Toxicol. 46 (S75-S82), 2008) . It has been shown that Rebaudioside A can transform from one polymorph to another under certain conditions (Ped. De Pat. US 11 / 556.049) as summarized in Table 3. Therefore, processes employed in the manufacture of Rebaudioside A should minimize the formation of forms with unwanted characteristics. Many agglomeration techniques that allow the contact of a solvent with a Rebaudioside A can facilitate the formation of solvate forms with undesirable characteristics. In the case of water or a solution or mixture containing water that comes into contact with Rebaudioside A, a hydrate form can be obtained which is characterized as the form with the lowest solubility.
    Table 3
    Properties of Rebaudioside A forms (US Pat. 11 / 556,049)
    Polymorphous Forms Form 1Hydrate Form 2 Animaldrosa Form 3 Solvate Form 4Amorphous Dissolution rate in H 2 O at 25 ° C Very low(<0.2% in 60minutes) Intermediate (<30% in 5 minutes) High (> 30% in5 minutes) High (> 35% in5 minutes) Alcohol content <0.5% <1% 1.3% <0.05% Moisture content > 5% <1% <3% 6.74%
    In addition, many processes employ binding agents or other auxiliary compounds that appear in the final product, thereby undesirably reducing the main ingredient content.
    There is, therefore, a significant need for a manufacturing process for granulated or agglomerated Rebaudioside A or other steviol glycosides having desirably high solubility and containing a significant or maximized amount or concentration of the main compound.
    US Patent Application 10 / 108,561 describes a method of producing granules of
    7/16 corn starch combining the starch with granulation fluid, submitting the mixture to wet sieving, drying and grading by size. It is noted that the addition of granulation fluids in the case of Stevia and Rebaudioside A sweeteners will facilitate the formation of low solubility polymorphs, which in turn will reduce the total solubility of the final composition.
    US Patent Application 11 / 873,610 provides a method of producing the granulated sweetener composition comprising poorly soluble polyol and hydrogenated dextrin. It is noted that the inclusion of auxiliary compounds in a composition reduces the active ingredient content.
    US Patent Application 11 / 979,530 describes a method for producing powder granules by subjecting them to the compaction force to produce a compacted mass comprising a mixture of particles and fine granules and separating the fine particles from the granules by attracting the fine particles in a gas stream.
    US patent 6,706,304 describes a method of preparing granular sweeteners comprising Aspartame and Acesulfame K as active ingredients. The mixture of ingredients was fed to the roller compactor granulator to obtain a granulated sweetener composition. It is noted that due to the sweetener polymorphism of Stevia and rebaudioside A, forms of low solubility can be formed during such a process that will result in a final composition with an undesirably low solubility.
    Summary of the Invention
    The invention is directed to a method for producing a sweetener comprising the steps of providing a Stevia sweetener powder, reducing the particle size of Stevia sweetener powder, treating Stevia sweetener powder under reduced pressure and elevated temperature, cooling the sweetener powder Stevia treated; and keeping the high solubility Stevia sweetening powder at low temperature to obtain a high solubility Stevia sweetening powder with increased solubility.
    Then, unless otherwise specified, the solubility of a material is determined in reverse osmosis water at room temperature. Where solubility is expressed as%, it should be understood as the number of grams of material soluble in 100 grams of solvent.
    The invention is similarly directed to a roller compaction method of a sweetener, starting with a high solubility sweetener powder, and introducing the high solubility sweetener powder to a roller compaction apparatus to produce a compacted material, introducing the compressed material to a size reduction apparatus to obtain a mixture of granules, and fractionating the mixture of granules by sieves of various sizes to obtain a granulated Stevia sweetener.
    The invention also includes a high solubility Stevia sweetener powder, and a granulated Stevia sweetener.
    It is to be understood that the foregoing general description and the following detailed description are exemplary and explanatory and are intended to provide another explanation of the invention as claimed.
    Brief Description of Drawings
    The accompanying drawings are included to provide another understanding of the invention. The drawings illustrate modalities of the invention and together with the description serve to explain the principles of the modalities of the invention.
    FIG. 1 shows the particle size distribution of a high solubility Rebaudioside A powder made according to an embodiment of the invention.
    Detailed Description of the Invention
    A process for granulating a Stevia sweetener, particularly Rebaudioside A, is described here. The process includes the steps of reducing the particle size of a Rebaudioside A composition, drying the Rebaudioside A particles using a heat treatment process, keeping the Rebaudioside A particles under nitrogen gas, compacting the particles, then granulating them to a desired mesh size. The resulting Rebaudioside A composition shows superior solubility and handling performance compared to other Rebaudioside A compositions. Although the following description describes Rebaudioside A, it should be understood that the processes and methods described here are also suitable for use with any type of Stevia sweetener.
    Rebaudioside A crystalline has an inherently very low solubility, ranging from about 1% -2%. As described above, Rebaudioside A exhibits polymorphism, resulting in a variety of shapes with very different characteristics and handling properties. The hydrate form has very low solubility (less than 0.2%), and is therefore not commercially viable as a sweetener. The solvate form has a solubility typically greater than 30%, but this form is only of scientific interest and cannot be used for food or drink applications because the residual alcohol level (1-3%) becomes unsuitable for use in food and drinks. The anhydrous form has a solubility reported in the literature of a maximum of up to about 30% solubility. The amorphous form generally has a solubility of more than 35%, but in the refining process, the amorphous form has to be dissolved in water and spray dried. The spray drying process requires the use of very diluted solutions, and spray drying itself is a very high energy consumption process, so this is not a viable option for the commercial production of Rebaudiosídeo A.
    The need exists, therefore, for a process in which a high solubility Rebaudioside A is obtained by a process that does not require significant dilution or a level
    5/16
    There are several publications on the purification of some individual steviol glycosides.
    Several patents describe the general process that can be used to prepare an extract of Stevia: Pat. No. 3,723,410; Pat. No. 4,082,858; Pat. No. 4,171,430; Pat. No. 4,361,697; Pat. No. 4,599,403; Pat. No. 4,892,938; Pat. No. 5,112,610; Pat. No. 5,962,678; Pat. No. 5,972,120; Pat. No. 6,031,157; Pat. No. 6,080,561; Pat. No. 7,807,206; and JP No. 01-131191; each of which is incorporated here by reference in its entirety.
    Generally, the production of a Stevia extract includes the extraction of plant material with water or a mixture of organic water solvent, precipitation of high molecular weight substances, deionization, and discoloration, purification in specific macroporous polymeric absorbents, concentration and drying.
    Leaf glycosides can be extracted using water or organic solvent extraction. Supercritical fluid extraction and steam distillation have also been described. Methods for recovering sweet Stevia rebaudiana diterpene glycosides using membrane technology, and organic solvents or water, such as methanol and ethanol, are also described in the literature.
    Stevia extract is dried by spray drying and / or vacuum drying technology to evaporate moisture and process the extract solvents. The resulting powder contains very fine particles with a very low moisture content and low volumetric density, which becomes too dry to handle during the food application process.
    To overcome the issues associated with very fine particle size and dust, agglomeration technology is used to reduce the dangerous nature of dust particles and their associated handling difficulties. However, most industrial agglomeration technologies require the use of a binder, which can be water or a solution of adhesive molecules.
    Using wet agglomeration technology, in which the wet binding component is used, it can adversely affect the physical and chemical characteristics of Stevia molecules, especially the solubility of Stevia extract. The present invention can provide a physical form of a Stevia sweetener product that is much more user friendly and reduces dust or fines, without substantially changing the physical and chemical characteristics of the different Stevia sweetener molecules.
    To enhance the sweetness profile and reduce the residual taste of high intensity sweeteners, one or more co-ingredients can be combined for specific food and beverage applications. This invention also helps in the release of the high intensity sweetener and one or more co-ingredients together in a proportion calibrated in a granulated particle form that is friendly to the process and the user.
    Due to the physicochemical properties of Stevia sweeteners, not all energy techniques are high, and that does not result in a product having unacceptably high levels of alcohol. The process of the present invention achieves these objectives by creating a form of Rebaudioside A with a high level of solubility, but without the concomitant dilution, cost, or high alcohol content associated with other processes.
    In one embodiment of the present invention, a starting material, comprising sweet glycosides from the Stevia rebaudiana Bertoni plant extract, which includes Stevioside Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside E, Rebaudioside F, Steviolbioside, Dulcoside A, Rubusoside and / or one mixing of them was subjected to particle size reduction to produce a powder with average particle size between about 20-60 pm, preferably between about 25-40 pm. The powder with a particle size less than 20 pm exhibits low fluidity reducing the efficiency of the process, considering that particles greater than 60 pm provide a product with low solubility. Any device that can reduce a particle size of a solid substance, such as a rotary mill, ball mill, sprayer and others, can be used for this process.
    The powder thus obtained is subjected to a heat treatment process under vacuum at a pressure of about 1-10000 Pa (0-100 mbar), preferably between about 5001500 Pa (5-15 mbar). The duration of the heat treatment can be between approximately 1-24 hours, preferably between approximately 2-6 hours. The temperature of the heat treatment is between about 90-130 ° C, preferably between about 100-110 ° C. The powder is subjected to heat treatment for a period of time and at a temperature sufficient to remove all water from the material, without significant product degradation.
    Upon completion of the heat treatment, the pre-heated nitrogen is introduced into the vacuum chamber to equal the pressure in the chamber with ambient pressure. The temperature of the preheated nitrogen in this nitrogen maintenance step is about 5 ° C lower than the heat treatment temperature. The vacuum chamber is connected to an orifice that prevents excessive pressure from forming. The nitrogen flow is maintained at a speed equal to 1/10 of the volume of the vacuum chamber per minute. The nitrogen temperature is gradually decreased to about 25 ° C over a period of between about 3-12 hours, preferably between about 4-6 hours. Nitrogen maintenance conditions are selected to provide smooth and uniform cooling conditions. Although nitrogen is described, any other substantially inert gas that will not hydrate, oxidize or otherwise chemically affect the product, can be used.
    In one embodiment, the high solubility powder was kept under nitrogen at a temperature between about 10-50 ° C, preferably between about 10-30 ° C. A temperature below 10 ° C was found to result in the condensation of ambient moisture in the product also in the process, resulting in the hydrated form of low solubility of
    10/16
    Rebaudioside A. If the powder was treated with a temperature higher than 50 ° C, it resulted in an overheated compacted mass during roller compaction that quickly cooled to room temperature after compaction and provided a Rebaudioside A product with low solubility.
    The purpose of this process is to obtain a polymorph form of Rebaudioside A with a high solubility. The high solubility Rebaudioside A powder obtained by this process has a solubility that is greater than about 30%, or is preferably at least about 35% or at least about 40%.
    As discussed above, the conventionally prepared anhydrous form of Rebaudioside A demonstrates a solubility of up to about 30%, and the amorphous form demonstrates a solubility that can be greater than 35%, but must be significantly diluted and spray dried when refined. Prior to the present invention, it was not possible to provide a high solubility form of Rebaudioside A that is stable, easy to refine on a large scale, and does not require spray drying or other dilution processes during a commercial refinement process. It was surprisingly found that using the process of the present invention, including thermally treating a Rebaudioside A powder under vacuum and keeping the powder under nitrogen gas, followed by granulation compaction and dry roller compaction, a stable, but very highly soluble form of Rebaudioside A can be produced.
    While not claiming to be bound by theory, it is believed that the high solubility form of Rebaudioside A made by the present invention is an anhydrous form of Rebaudioside A having significantly improved solubility properties when compared to a conventional anhydrous form of Rebaudioside A, and that can be refined to a granular form without the dilution or spray drying required to refine the amorphous form of Rebaudioside A.
    The granulation refines to high solubility Rebaudioside A powder in a form suitable for handling and for industrial or consumer use. Dry granulation provides numerous advantages over wet agglomeration, such as being a continuous process capable of internally recycling granules out of specification, requiring no additional bonding materials, and not requiring an additional drying step once the product is granulated.
    A granulation method is using roller compaction in which the powder is fed to two counter-rotating rolls that pull the powder between the rolls due to friction and compact the powder into a sheet or layer of material. Roller compaction inherently reduces the solubility of materials. Therefore, when reaching a desirable level of solubility in a granulated product, it is desirable to have a starting material with a high solubility rate before compaction, so that the resulting compacted and granulated material has the highest possible solubility for a given material.
    The granulated material made according to the present invention advantageously produces a product with favorable characteristics such as solubility, particle size distribution and purity. In fact, it has been found that the dissolution rate of the high solubility Rebaudioside A granular particles of the present invention is actually higher, and still significantly higher, than the dissolution rate of the high solubility Rebaudioside A powder before roller compaction . While not intending to be bound by theory, it is believed that the granulation process of the present invention improves the dispersibility of high solubility Rebaudioside A, resulting in a faster dissolution rate.
    During compaction, if the roller pressure is too low, it can result in the formation of loose granules with poor mechanical stability. If the roller pressure is too high, it may result in overcompacted material that has a slower dissolution rate. In one embodiment of the present invention, the speed of the roller was between about 5-20 rpm, preferably between about 7-10 rpm, and more preferably about 9 rpm. The roller pressure was between about 10x10 5 -60x10 5 Pa (10-60 bar), preferably between about 30x10 s -50x10 5 Pa (30-50 bar), and more preferably about 45x10 5 Pa (45 bar) .
    Numerous factors affect the solubility of a dry material, including the density of the material. It has been found that suitable density values that provide the desired solubility values range from about 0.35 to about 0.45 g / cc after roller compaction.
    The compressed Rebaudioside A material can then be processed by a granulation apparatus. In one embodiment, the apparatus contained two granulators, a pre-granulator and a fine granulator. The purpose of granulators is to generate granules of compacted material produced by the roller compactor. Each granulator is equipped with rotors that press the coarse material through a U-shaped screen. If the screen size is too small, it results in an excessive amount of fine particles. If the screen size is very large, it produces large particles with a lower dissolution rate.
    In one embodiment, the rotors were rotating at a rate of between about 50,000 rpm, preferably between about 100-200 rpm, and more preferably at about 150 rpm. The granulators were equipped with screens whose sizes were between about 0.5-6.0 mm, preferably between about 1-4 mm, and more preferably about 3.1 mm for the pre-granulator and about 1.6 mm for the fine granulator.
    The product of Rebaudioside A granulate resulting from this modality was fractionated in the mesh of US ## 8 mesh; 10; 14; 20; 40 and 60. The results are presented in the
    12/16
    Table 4.
    Table 4
    Particle size distribution
    US mesh # % withheld 8 0 10 0.1 14 26.3 20 39.5 40 24.8 60 6.5
    About 2.8% of the material passed through the US # 60 mesh sieve.
    The sweetener of Rebaudioside A granulate obtained by the method of the present invention has a solubility ranging from about 1.0% to more than 40%.
    In one embodiment of the invention, the high solubility Rebaudioside A powder can be mixed with other ingredients to form a mixture of Rebaudioside A prior to granulation. The high solubility Rebaudioside A powder is capable of being mixed with other ingredients to achieve the proper distribution of all ingredients in the final product. Non-limiting examples of other ingredients that can be combined with high solubility Rebaudioside A powder before granulation include: natural and synthetic high intensity sweeteners as previously described; natural sweeteners such as sucrose, fructose, glucose, maltose, lactose, tagatose, and palatinose; sugar alcohols such as erythritol; taste-modifying agents such as condiments and extracts; flavor modifying agents such as thaumatin, glycyrrhizin, Rebaudioside C, and Rebaudioside D; bulking agents or mouthfeel modifiers such as Fibersol®, soluble corn fiber, Arabica form, pectin, isomaltooligosaccharide; and combinations thereof.
    It was found that by balancing the use of other ingredients in combination with Rebaudioside A, the taste and weather profiles of the resulting sweetener can be improved. For example, while not pretending to be bound by theory, it is believed that the use of a very small amount of a flavor-modifying agent can serve to saturate or block specific taste buds during the early part of consumption, thereby making these taste buds unavailable for transmitting specific flavor signals to the brain while consuming the rest of the drink or food. The flavor modifying agent itself can have a very high degree of the particular taste, such as bitterness, which must be blocked by saturating the receptors on the tongue with this flavor.
    The sweetness profile of Rebaudioside A can be increased in the same way with
    13/16 the use of sugar, such as cane or beet sugar. Although the sugar and Stevia sweeteners have different melting characteristics and solubility, it is believed that the use of the dry roll compaction granulation process of the present invention results in a sweetener composition containing reduced calorie sugar that is uniform and provides a uniform consistent dispersion when used in a food or drink application.
    The following examples illustrate various embodiments of the invention. It will be understood that the invention is not limited to the materials, proportions, conditions and procedures mentioned in the examples, which are illustrative only.
    Example 1
    Preparation of high solubility Rebaudioside A
    100 kg of Rebaudioside A, containing Stevioside 0.2%, Rebaudioside C 0.2%,
    Rebaudioside F 0.3%, Rebaudioside A 97.5%, Rebaudioside D 1.1%, Rebaudioside B 0.5%, all percentages based on the dry weight percentage, and having 1.6% water solubility were placed in a rotary blade grinding machine and pul15 checked for 20 minutes. The resulting powder was analyzed by Beckman Coulter LS 13 320 Laser Diffraction Particle Size Analyzer. The results are summarized in Table 5.
    Table 5
    Results of Powder Laser Diffraction Analysis
    Operation mode Volume statistics Calculations: from 0.375 pm to 2000 pm Average: 31.07 pm Median: 23.11 pm Average / Average Ratio: 1,344 Mode: 50.22 pm S.D .: 27.15 pm Variance: 737.4 pm 2 C.V .: 87.4% Distribution <10% 3,356 pm <25% 10.11 pm <50% 23.11 pm <75% 45.76 pm <90% 70.19 pm
    The obtained powder was loaded in a 1000 L rotary vacuum dryer and dried at 105 ° C at a pressure of 1000 Pa (10 mbar) for 3 hours. After 3 hours, nitrogen
    14/16 preheated to 100 ° C was introduced into the vacuum chamber until ambient pressure is reached. Upon reaching room pressure, the vacuum dryer was connected to an orifice and the nitrogen flow was continued at 100 L / min over a 4 hour period. The temperature of the nitrogen gas was gradually decreased by decreases of 5 ° C until reaching 25 ° C over the course of the 4 hour time period. A sample of the powder was taken from the dryer and the solubility tested in deionized water at room temperature. The solubility was 41.1%, and the dissolution time was 7 minutes. The particle size distribution of the high solubility Rebaudioside A powder is shown in FIG. 1.
    Example 2
    Granulation of Rebaudioside A kg of high solubility Rebaudioside A prepared according to example 1 was placed in a 500L double cone shaped powder mixer and nitrogen at 10 ° C was fed to the container for 1 hour. The powder was transferred to the Alexanderwerk WP 50N / 75 roller compactor. The compactor was operating at 9 rpm and a pressure of 45x10 5 Pa (45 bar). The compacted mass was fed to a pre-granulator and a fine granulator with rotors rotating at 150 rpm. The screen size for the pre-granulator was 3.1 mm and for the fine granulator it was 1.6 mm. The "overs (particles that are very large) and" fines "(particles that are very small) were separated by an upper screen having a mesh size of US 10 mesh and a lower mesh of US 40 mesh. 0% ratio of" overs "":" Product ":" fines "was 0.3%: 72.1%: 27.6% respectively.
    Example 3
    Granulation of Rebaudioside A kg of high solubility Rebaudioside A prepared according to example 1 were granulated according to the procedure of example 2. The compactor was operating at 18 rpm and a pressure of 65x10 5 Pa (65 bar). The compacted mass was fed to a pre-granulator and a fine granulator with rotors rotating at 300 rpm. The screen size for the pre-granulator was 5 mm and for the fine granulator it was 3 mm.
    Example 4
    Granulation of Rebaudioside A kg of high solubility Rebaudioside A prepared according to example 1 were granulated according to procedure of example 2. The compactor was operating at 9 rpm and a pressure of 45x10 5 Pa (45 bar). The compacted mass was fed into a pre-granulator and fine granulators with rotors rotating at 150 rpm. The screen size for the pre-granulator was 2 mm and for the fine granulator it was 0.5 mm. The "overs and" fines were separated by an upper mesh of US # 10 mesh and a lower mesh of US # 40 mesh. Product yield was 34%, considering that 66% of product passed through US # 40 mesh. Subsequent sieving of the material that passed through US # 40 mesh through a Ma15 / 16 ml US # 80 sieve resulted in 28% of powder passing through US # 80 mesh.
    Example 5
    High Solubility Rebaudioside A Dissolution Rate
    Four batches of high solubility Rebaudioside A powder were used to prepare the granulated product using the roller compaction technology as described above. All granulated and powder samples were tested for their solubility and dispersion time. The test was administered by adding 5.0 g of high solubility Rebaudioside A granules or powder in 500 ml of water at room temperature. The mixture was then stirred with a magnetic stirrer to create a significant vortex for the mixture itself. The dissolution rate was timed on a timer starting as soon as the high solubility Rebaudioside A was added directly to the stirred water. The data, summarized in Table 6, showed that the granulation shortened the dissolution time (the time to have the clear solution) without any loss of solubility.
    Table 6
    Dissolution Times and Rates of High Solubility Rebaudioside A Powder Dust and Granular Form
    Hitlada Dissolution Time (Powder) Rate ofDissolution(Powder) Dissolution Time (Granular) Dissolution Rate(Granular) % inIncreaseRateof Dust 1 7 min 11 seconds 0.70 g / min 6 min 35 seconds 0.76 g / min 8.6% 2 10 min 5 seconds 0.50 g / min 4 min 41 seconds 1.07 g / min 114% 3 8 min 35 seconds 0.58 g / min 5 min 36 seconds 0.90 g / min 55% 4 13 min 12 seconds 0.38 g / min 5 min 11 seconds 1.00 g / min 163%
    The process of the present invention resulted in a single polymorph of Rebaudioside A that demonstrated an unexpectedly higher degree of water solubility than other polymorphic forms. Although the foregoing embodiments describe the use of Rebaudioside A, it should be understood that any Stevia-based sweetener can be used and prepared in accordance with this invention, and all Stevia-based sweeteners are considered to be within the scope of the present invention.
    Although the invention and its advantages have been described in detail, it should be understood that various changes, substitutions and changes can be made here without departing from the spirit and scope of the invention as defined by the appended claims.
    16/16
    Furthermore, it is not intended that the scope of the application be limited to the particular embodiments of the invention described in the specification. Since someone with ordinary experience in the technique will easily show from the description of the invention, the compositions, processes, methods, and steps, now existing or later to be developed which perform the same function or achieve substantially the same result as the modalities corresponding described herein can be used according to the invention.
    1/2
    权利要求:
    Claims (11)
    [1]
    1. Method to produce a sweetener CHARACTERIZED by understanding the steps of:
    A) provide Stevia sweetener powder;
    B) reducing the particle size of the Stevia sweetener powder to a particle size of 20pm to 60pm;
    C) treat Stevia sweetener powder under reduced pressure of 0-10000 Pa (0mbar at 100 mbar) and elevated temperature from 90 ° C to 130 ° C;
    D) cool the treated Stevia sweetener powder to a low temperature of 25 ° C;
    10 E) keep the Stevia sweetening powder cooled at low temperature to obtain a high solubility Stevia sweetening powder with increased solubility of at least 30 g per 100g of water; and
    F) introducing the Stevia sweetener powder of high solubility to a roller compaction apparatus to produce a compacted material;
    G) introducing the compacted material to a size reduction apparatus to obtain a mixture of granules; and
    H) fractionating the granule mixture through sieves of various sizes to obtain a granulated Stevia sweetener having a particle size ranging from 0.425 mm to 2.0 mm and having a higher dissolution rate than the dissolution rate of Stevia powder in
    20 high solubility.
    [2]
    2. Method, according to claim 1, CHARACTERIZED by the fact that the dissolution rate of the granulated Stevia sweetener is 0.75 grams per minute to 1.07 grams per minute.
    [3]
    3. Method, according to claim 1, CHARACTERIZED by the fact that Stevia sweetener is selected from a group consisting of: Stevioside, Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside D, Rebaudioside E, Rebaudioside F, Steviolbioside , Dulcoside A, Rubusoside, or a mixture of these.
    [4]
    4. Method, according to claim 1, CHARACTERIZED for cooling the treated Stevia powder comprises introducing preheated nitrogen gas into a vacuum chamberPetition 870170074341, of 10/02/2017, p. 12/13
    2/2 cuo and gradually reduce the temperature of the nitrogen gas.
    [5]
    5. Method, according to claim 1, CHARACTERIZED by the fact that the compaction device operates between 5 rpm and 20 rpm, and at a roller pressure between 10x10 5 Pa and 60x10 5 Pa (10 bar and 60 bar) to produce the compacted material; and the size reduction apparatus comprises a set of sequentially located granulating equipment equipped with rotors rotating between 50 rpm and 2000 rpm.
    [6]
    6. Method, according to claim 1, CHARACTERIZED by the fact that Stevia sweetener powder is selected from a group consisting of: Stevioside, Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside D, Rebaudioside E,
    10 Rebaudioside F, Steviolbioside, Dulcoside A, Rubusoside, or a mixture of these.
    [7]
    7. Method according to claim 1, further comprising the step of combining Stevia sweetener powder with an additional ingredient before introducing the powder to the roller compaction apparatus.
    [8]
    8. Method, according to claim 7, CHARACTERIZED by the fact that the additional ingredient is selected from the group consisting of: a high intensity sweetener; a natural sweetener; a sugar alcohol; a flavoring agent; a flavor modifying agent; a taste-modifying agent; a bulking agent; or a combination of these.
    [9]
    9. Method, according to claim 5, CHARACTERIZED by the fact that the legs comprise U-shaped screens having opening sizes ranging from 0.5 mm to 6.0 mm.
    [10]
    10. Method according to claim 5, CHARACTERIZED by comprising a first granulator and a second granulator, said first granulator being equipped with a U-shaped screen having an opening size of 3.1 mm and the reference of the second granulator being equipped with a U-shaped screen having an opening size of 1.6 mm.
    [11]
    11. Method, according to claim 1, CHARACTERIZED by the fact that the dissolution rate of the granulated Stevia sweetener is 8.6% to 163% higher than the dissolution rate of the high solubility Stevia powder.
    Petition 870170074341, of 10/02/2017, p. 13/13
    1/1
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    法律状态:
    2017-07-04| B07A| Technical examination (opinion): publication of technical examination (opinion)|
    2017-11-07| B09A| Decision: intention to grant|
    2018-02-06| B16A| Patent or certificate of addition of invention granted|
    2018-03-27| B15K| Others concerning applications: alteration of classification|Ipc: A23C 9/13 (2006.01), A23G 3/36 (2006.01), A23G 3/4 |
    优先权:
    申请号 | 申请日 | 专利标题
    US26046509P| true| 2009-11-12|2009-11-12|
    US26059309P| true| 2009-11-12|2009-11-12|
    US61/260.593|2009-11-12|
    US61/260.465|2009-11-12|
    US29077809P| true| 2009-12-29|2009-12-29|
    US61/290.778|2009-12-29|
    US12/720,888|US8334006B2|2005-10-11|2010-03-10|Process for manufacturing a sweetener and use thereof|
    US12/720.888|2010-03-13|
    US12/753.470|2010-04-02|
    US12/753,470|US8337927B2|2005-10-11|2010-04-02|Process for manufacturing a sweetener and use thereof|
    PCT/US2010/055960|WO2011059954A1|2009-11-12|2010-11-09|Granulation of a stevia sweetener|
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