Patent ID: 12193460

DETAILED DESCRIPTION OF THE INVENTION

A process for the preparation of highly solubleSteviasweetener, particularly Rebaudioside M composition, is described herein.

Crystalline Rebaudioside M has an inherently very low solubility, ranging from about 0%-0.1%.

Typical spray drying techniques are used to increase the solubility of steviol glycosides compositions. However the heat applied in spray drying may cause thermal degradation of material a reducing its purity below legally permitted levels. Therefore there's a need to develop a new method of increasing the solubility of steviol glycosides with minimal heat exposure and heat degradation.

In one embodiment of the present invention, an initial material, comprising sweet glycoside(s) occurring inStevia rebaudianaplant, which includes Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside D, Rebaudioside E, Rebaudioside F, Rebaudioside G, Rebaudioside H, Rebaudioside I, Rebaudioside J, Rebaudioside K, Rebaudioside L, Rebaudioside M, Rebaudioside N, Rebaudioside O, Rebaudioside Q, Stevioside, Steviolbioside, Dulcoside A, Rubusoside, or other glycoside of steviol and combinations thereof was combined with the water.

The obtained mixture was further subjected to heating which resulted in steviol glycosides solution. The mixture was heated to the temperature of 50-110° C., preferably 80-100° C. and was held at maximum temperature for 0-120 sec, preferably 1-10 sec.

After the heat treatment the solution was quickly cooled down to below freezing temperature. In one embodiment the mixture was cooled to the temperature −1° C. to −200° C., preferably −24° C. to −196° C.

The frozen solution was freeze dried by laboratory freeze dried until <1% water content. A highly soluble amorphous form of rebaudioside M was obtained having 2% solubility in water at room temperature.

The process of the present invention resulted in a Rebaudioside M composition which demonstrated high degree of solubility in water. Although the foregoing embodiments describe the use of Rebaudioside M, it is to be understood that any composition comprising at least one steviol glycosides and having water solubility of 0.1% and less may be used as starting material to prepare highly soluble steviol glycosides composition having water solubility of 0.5% and more in accordance with this invention. Particularly highly soluble steviol glycosides compositions of present invention can have water solubility not less than 0.5% 0.6%, 0.7%, 0.8% 0.9%, 1.0%, 1.1%, 1.2%, 1.3%, 1.4%, 1.5%, 1.6%, 1.7%, 1.8%, 1.9%, 2%, 3%, 4%, 5%, 6%, 9%, 10%. The compositions can be used as sweetener, sweetness enhancer, flavor enhancer sweetness modifier, flavor modifier in various food and beverage products at the concentration from 0.1 ppm to 999,999 ppm. Non-limiting examples of food and beverage products include carbonated soft drinks, ready to drink beverages, energy drinks, isotonic drinks, low-calorie drinks, zero-calorie drinks, sports drinks, sodas, colas, teas, fruit and vegetable juices, juice drinks, dairy drinks, yoghurt drinks, alcohol beverages, powdered beverages, bakery products, cookies, biscuits, baking mixes, cereals, confectioneries, candies, toffees, chewing gum, dairy products, flavored milk, yoghurts, flavored yoghurts, cultured milk, soy sauce and other soy base products, salad dressings, mayonnaise, vinegar, frozen-desserts, meat products, fish-meat products, bottled and canned foods, tabletop sweeteners, fruits and vegetables.

Additionally the compositions can be used in drug or pharmaceutical preparations and cosmetics, including but not limited to toothpaste, mouthwash, cough syrup, chewable tablets, lozenges, vitamin preparations, and the like, at the concentration from 0.1 ppm to 999,999 ppm.

The obtained compositions can be used “as-is” or in combination with other sweeteners, flavors and food ingredients.

Non-limiting examples of sweeteners include at least one sweetener selected from group including steviol glycosides, Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside D, Rebaudioside E, Rebaudioside F, Rebaudioside G, Rebaudioside H, Rebaudioside I, Rebaudioside J, Rebaudioside K, Rebaudioside L, Rebaudioside M, Rebaudioside N, Rebaudioside O, Rebaudioside Q, Stevioside, Steviolbioside, Dulcoside A, Rubusoside, or other glycoside of steviol and combinations thereof, glycosylated steviol glycosides, glucosylated steviol glycosides, fructosylated steviol glycosides, galactosylated steviol glycosides, enzymatically modified steviol glycosides as well as other steviol glycosides found inStevia rebaudianaplant and mixtures thereof, stevia extract, Luo Han Guo extract, mogrosides, high-fructose corn syrup, corn syrup, invert sugar, fructooligosaccharides, inulin, inulooligosaccharides, coupling sugar, maltooligosaccharides, maltodextrins, corn syrup solids, glucose, maltose, sucrose, lactose, aspartame, saccharin, sucralose, sugar alcohols.

Non-limiting examples of flavors include at least one flavor selected from the group including lemon, orange, fruit, banana, grape, pear, pineapple, bitter almond, cola, cinnamon, sugar, cotton candy, vanilla flavors, terpenoid glycosides and/or combinations thereof.

Non-limiting examples of other food ingredients include at least one selected from group of flavors, acidulants, organic acids, amino acids, coloring agents, bulking agents, modified starches, gums, texturizers, preservatives, antioxidants, emulsifiers, stabilisers, thickeners, caffeine, gelling agents and/or combinations thereof.

The following examples illustrate preferred embodiments of the invention. It will be understood that the invention is not limited to the materials, proportions, conditions and procedures set forth in the examples, which are only illustrative.

EXAMPLE 1

Preparation of Steviol Glycosides Concentrated Solution

5 g of rebaudioside M produced by PureCircle Sdn Bhd (Malaysia) containing Rebaudioside M 83.2%, Rebaudioside D 10.5%, Rebaudioside A 1.5%, Stevioside 0.1%, Rebaudioside B 0.95%, all percentages being on a percent dried weight basis, and having water solubility of 0.05% was mixed with 50 g of water and boiled on a laboratory heater until complete dissolution.

EXAMPLE 2

Preparation of Spray Dried Highly Soluble Steviol Glycosides

Rebaudioside M solution prepared according to EXAMPLE 1, was dried using YC-015 laboratory spray drier (Shanghai Pilotech Instrument & Equipment Co. Ltd., China) operating at 175° C. inlet and 100° C. outlet temperature to yield Sample #1.

EXAMPLE 3

Preparation of Steviol Glycosides Frozen Solution

The beaker with Rebaudioside M solution prepared according to EXAMPLE 1, was transferred directly from heater to laboratory freezer operating at −24° C. Upon complete solidification the obtained frozen solution A was placed in liquid nitrogen.

EXAMPLE 4

Preparation of Steviol Glycosides Frozen Solution

The beaker with Rebaudioside M solution prepared according to EXAMPLE 1, was transferred directly from heater into to liquid nitrogen. Upon complete solidification the obtained frozen solution B was kept in liquid nitrogen.

EXAMPLE 5

Preparation of Freeze Dried Highly Soluble Steviol Glycosides

Rebaudioside M frozen solution A and frozen solution B prepared according to EXAMPLE 3 and EXAMPLE 4 were dried using ALPHA 1-4 LSC laboratory freeze drier (Martin Christ, Germany) until <1% water content. The frozen solution A yielded Sample #2, Solution #2 and frozen solution B yielded Sample #3.

The obtained highly soluble steviol glycosides samples and initial crystalline material were compared for solubility (Table 2) and were subjected to HPLC assay for steviol glycoside content analysis (Table 3).

TABLE 2Highly soluble steviol glycosidesTurbidity (FAU)SolubilityInitial crystallineat % w/wReb MSample#1Sample#2Sample#30.05100000.5Unreadable9701%Unreadable141342%Unreadable21169

TABLE 3HPLC assay of soluble steviol glycosidesHPLC Assay % w/wSample IDRebDRebMRebAStevRebBTSGInitial crystalline Reb M10.4883.251.460.100.9596.24Sample #110.0980.371.380.101.5893.52Sample #210.4283.231.480.100.9796.20Sample #310.4383.261.450.100.9596.19

The HPLC data suggests thermal degradation of Sample #1. Sample #2 and Sample #3 show no degradation of steviol glycosides and better solubility in water.

Although the invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims. Moreover, the scope of the application is not intended to be limited to the particular embodiments of the invention described in the specification. As one of ordinary skill in the art will readily appreciate from the disclosure of the invention, the compositions, processes, methods, and steps, presently existing or later to be developed that perform substantially the same function or achieve substantially the same result as the corresponding embodiments described herein may be utilized according to the invention.