巴西专利BR112013020513B1 method for producing a soluble stevia sweetener

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专利摘要:
Highly Soluble Stevia Sweetener A method for producing highly soluble stevia sweetener is provided. The resulting sweetener quickly provides solutions with up to or above 30% concentration that are stable for more than 24 hours.
公开号:BR112013020513B1
申请号:R112013020513-0
申请日:2012-02-10
公开日:2019-10-29
发明作者:Markosyan Avetik
申请人:Markosyan Avetik；Purecircle Usa Inc；
IPC主号:

专利说明:

"METHOD FOR THE PRODUCTION OF A SOLUBLE STEVIA SWEETENER"
FIELD OF THE INVENTION
The present invention relates to a process for the preparation of highly soluble sweet glycosides individually or combined from an extract of the plant Stévia rebaudiana Bertoni, and more particularly for the preparation of highly soluble Rebaudioside A.
DESCRIPTION OF THE PREVIOUS TECHNIQUE
It is common knowledge that Rebaudiosídeo A presents the so-called polymorphism (Zell et al., 2000). The amorphous, anhydrous and dissolved forms of Rebaudioside A are significantly different from each other in terms of solubility, which is one of the main criteria for the commercial viability of a sweetener. In this regard, as shown in Table 1, the hydrate form of Rebaudioside A has the lowest solubility (Prakash et al., 2008). It has been shown that Rebaudioside A can change from one polymorph to another under certain conditions (US Patent Application 11 / 556,049).
Table 1
Form 1 Hydrate Anhydrous Form 2 Form 3 Solvate Amorphous Form 4 Dissolution rate in H2O 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%
Patent application WO / 2010/118218 describes a process for producing highly soluble Rebaudioside A by preparing a highly soluble hydrated crystalline form. However, the methodology described uses low productivity techniques such as evaporation crystallization or hot sludge filtration / centrifugation which can be difficult to achieve on a large industrial scale.
On the other hand, it is known (Prakhash et al., 2008) that the amorphous forms of Rebaudioside A prepared by spray drying also exhibit high solubility. However, spray drying of Rebaudiosídeo A is a very challenging and low-productivity task because it usually requires concentrated feed solutions (about 50% solid content). Concentrated solutions of Rebaudioside A prepared by simple dissolution are very unstable and tend to crystallize very quickly. These concentrated solutions (> 10%) prepared by common solubilization methods, such as heating under normal conditions, crystallize shortly after cooling to room temperature. Thus, spray drying such solutions requires special equipment capable of maintaining the solution at an elevated temperature.
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On the other hand, prolonged exposure of Rebaudioside A to a high temperature in both solid form and aqueous solutions results in a hydrolytic decomposition of the material (Prakash et al., 2008).
Therefore, a highly productive process to manufacture highly soluble Rebaudioside A or other steviol glycosides on an industrial scale without requiring a configuration using sophisticated equipment will offer certain advantages compared to other techniques known in the field.
SUMMARY OF THE INVENTION
The present invention addresses a method for producing a sweetener comprising the steps of providing a Stévia sweetener powder and dissolving it in water under treatment conditions at a temperature gradient, to produce a highly stable concentrated solution, and spray-drying the highly stable concentrated solution to obtain a highly soluble Stévia sweetener powder.
Hereinafter the term “glycoside (s) steviol” will mean Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside D, Rebaudioside E, Rebaudioside F, Stevioside, Steviolbioside, Dulcoside A, Rubusoside, or other steviol glycoside and combinations thereof.
Henceforth, unless otherwise indicated, the solubility of material is determined in RO water (reverse osmosis) at room temperature. Where the solubility is expressed as "%" it must be understood as the number of grams of material soluble in 100 grams of solvent.
It is to be understood that both the general description offered and the detailed description below are exemplary and explanatory and are intended to provide a further explanation of the invention as claimed.
DETAILED DESCRIPTION OF THE INVENTION
A process for the preparation of highly soluble Stévia sweetener, particularly Rebaudioside A, is described here.
Crystalline Rebaudioside A has an inherently very low solubility, ranging from 1% -2%. As described above, Rebaudioside A exhibits polymorphism, which results 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 dissolved form has a solubility typically greater than 30%, but this form is of scientific interest only and cannot be used in food or beverage applications because the residual alcohol level (1-3%) makes it unsuitable for use in food and drinks. The anhydrous form has a solubility reported in the bibliography as a maximum solubility of 30%. The amorphous form has a solubility generally greater than 30%, but because of its preparation, the crystalline form has
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3/5 of being dissolved in water at very high concentrations (approximately 50%), which is not achieved by common dissolution techniques.
Typical spray drying techniques involve the use of a highly concentrated, yet stable, initial solution to achieve the highest possible productivity. As noted above, crystalline Rebaudioside A has very low solubility, so to create a stable solution (one that will not crystallize at room temperature), the solution has to be very diluted. Spray drying highly diluted solutions is not economically efficient because the production of spray dried powder will be very low. There is a need, therefore, for a process in which a Rebaudioside A with high solubility is obtained by a process that does not require a significantly diluted Rebaudioside A solution in order for the solution to be stable at room temperature.
In one embodiment of the present invention, a starting material comprising sweet glycoside (s) from the extract of the plant Stévia rebaudiana Bertoni, which includes Stevioside, Rebaudioside A, Rebaudioside B, Rebaudioside C, Rebaudioside D, Rebaudioside E, Rebaudioside F, Steviolbioside , Dulcoside A, Rubusoside, or another steviol glycoside and combinations thereof, was combined with water at a ratio of about 1: 1 (w / w).
The obtained mixture was also subjected to a thermal gradient treatment that resulted in a solution with high stability and high concentration. The gradient of about 1 ° C per minute was used to heat the mixture. The mixture was heated to a temperature of about 110-140 ° C, preferably about 118-125 ° C and was kept at the maximum temperature for about 0-120 minutes, preferably about 50-70 minutes.
After heat treatment the solution was cooled to room temperature at a gradient of about 1 ° C per minute. The 24-hour incubation of this high-stability, high-concentration solution showed no crystallization.
The solution was spray dried by a laboratory spray dryer operating at an inlet temperature of about 175 ° C and an outlet temperature of about 100 ° C. A highly soluble amorphous form of Rebaudioside A was obtained with a solubility greater than about 30% in water at room temperature.
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 shown in the examples, which are illustrative only.
EXAMPLE 1: Preparation of Rebaudioside A concentrated solution
100 grams of rebaudioside A containing 0.2% Stevioside, 0.3% Rebaudioside C, 0.3% Rebaudioside F, 97.7% Rebaudioside A, 1.0% Rebaudioside D, and 0.3% Rebaudioside B, all percentages being on a percentage basis of
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4/5 dry weight, and having a solubility in water of 0.6%, were mixed with 100 g of water and boiled in a laboratory heater until complete dissolution. Upon complete dissolution, the solution was cooled to room temperature to make Solution # 1.
EXAMPLE 2: Preparation of Rebaudioside A concentrated solution
100 g of rebaudioside A containing 0.2% Stevioside, 0.3% Rebaudioside C, 0.3% Rebaudioside F, 97.7% Rebaudioside A, 1.0% Rebaudioside D, and 0.3% of Rebaudioside B, all percentages being on a dry weight percentage basis, and having a solubility in water of 0.6%, were mixed with 100 g of water and incubated in an autoclave (AMA 270, Astell Scientific, UK) at 121 ° C for one hour. Upon completion of the incubation period, the clear solution obtained was cooled to room temperature to make Solution # 2.
EXAMPLE 3: Preparation of Rebaudioside A concentrated solution
100 g Rebaudioside A containing 0.2% Stevioside, 0.3% Rebaudioside C, 0.3% Rebaudioside F, 97.7% Rebaudioside A, 1.0% Rebaudioside D, and 0.3% of Rebaudiosídeo B, all percentages being on a dry weight percentage basis, and having a solubility in water of 0.6%, were mixed with 100 g of water and incubated in an oil bath with thermostat. The temperature was increased at 1 ° C per minute to 121 ° C. The mixture was kept at 121 ° C for one hour and then the temperature was lowered to room temperature (25 ° C) at 1 ° C per minute to make Solution # 3.
EXAMPLE 4: Stability of concentrated Rebaudioside A solution
Solution # 1, Solution # 2, and Solution # 3 of Rebaudioside A prepared according to EXAMPLE 1, EXAMPLE 2 and EXAMPLE 3, respectively, were evaluated in terms of their stability at room temperature (25 ° C). The results are summarized in Table 2.
Time, hours Note Solution # 1 Solution # 2 Solution # 3 0.5 Clear solution Clear solution Clear solution 1 Intensive Crystallization Blurred solution, precipitated at the bottom Clear solution 2 Viscous crystal mud Intensive Crystallization Clear solution 4 Solidified crystalline mixture Viscous crystal mud Clear solution 24 Solidified crystalline mixture Solidified crystalline mixture Clear solution
It can be seen that the solution prepared by the temperature gradient method shows greater stability against crystallization.
EXAMPLE 5: Preparation of highly soluble Rebaudioside A
Solution # 1, Solution # 2, and Rebaudioside A Solution # 3 prepared according to EXAMPLE 1, EXAMPLE 2 and EXAMPLE 3, respectively, were dried using the YC-015 laboratory spray dryer (Shanghai Pilotech Instrument &
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Equipment, Co. Ltd, China) operating at a temperature of 175 ° C at the inlet and 100 ° C at the outlet. Solution # 1 and Solution # 2 had to be kept at 80 ° C to avoid premature crystallization while Solution # 3 was kept at room temperature. Solution # 1 produced Sample # 1, Solution # 2 produced Sample # 2 and Solution # 3 produced Sample # 3.
The amorphous powder samples obtained were compared for solubility (Table 3).
Table 3
Solubility,% Note Sample # 1 Sample # 2 Sample # 3 5 Clear solution Clear solution Clear solution 10 Slightly cloudy solution Clear solution Clear solution 20 Blurred solution Slightly cloudy solution Clear solution 30 Undissolved matter at the bottom Blurred solution Clear solution 40 Significant amount of undissolved matter Significant amount of undissolved matter Slightly cloudy solution
The process of the present invention resulted in a polymorph of Rebaudioside A that demonstrated a high degree of solubility in water. Although the modalities presented describe the use of Rebaudioside A, it should be understood that any sweetener based on Stevia can be used and prepared according to that invention, and that all sweeteners based on Stevia are considered to be within the scope of this invention.
Although the invention and its advantages have been described in detail, it should be understood that various changes, substitutions and alterations can be made to it without departing from the spirit and scope of the invention as defined by the appended claims. Furthermore, it is not intended that the scope of the application be limited to the particular embodiments of the invention described in the report. As someone of average skill in the art will readily appreciate from the disclosure of the invention, the compositions, processes, methods and steps currently existing or to be further developed that perform substantially the same function or arrive at substantially the same result as the corresponding modalities described here may be used according to the invention.

权利要求:
Claims (8)
[1]
1. Method for producing a soluble Stévia sweetener, FEATURED by the fact that it comprises the steps of:
a) supply a Stévia sweetener powder;
b) supply water;
c) mix water and Stévia sweetener powder to make a mixture;
d) increasing the temperature of the mixture using a gradient heat treatment method at a gradient of about 1 ° C per minute to an elevated temperature of 110-140 ° C to make a solution;
e) keep the solution at an elevated temperature of 110-140 ° C; and
f) decrease the temperature of the solution using a gradient cooling method with a rate of change of temperature to obtain a soluble Stévia sweetener solution with a clear solution stability without visible crystallization or cloudiness at room temperature for 24 hours.
[2]
2. Method according to claim 1, CHARACTERIZED by the fact that it additionally comprises spray-drying the Stévia sweetener solution to provide an amorphous Stévia sweetener powder.
[3]
3. Method, according to claim 1, CHARACTERIZED by the fact that the sweetener Stévia 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 other steviol glycoside, and a mixture thereof.
[4]
4. Method, according to claim 1, CHARACTERIZED by the fact that the ratio of water to sweetener powder Stevia in the mixture is 1: 1 (w / w).
[5]
5. Method, according to claim 1, CHARACTERIZED by the fact that the mixture of water and sweetener Stévia is kept at about 110-140 ° C for about 5070 minutes.
[6]
6. Method, according to claim 1, CHARACTERIZED by the fact that the Stévia sweetener solution is spray-dried in a spray dryer operating at an inlet temperature of 175 ° C and an outlet temperature of 100 ° Ç.
[7]
7. Method, according to claim 1, CHARACTERIZED by the fact that the sweetener Stévia has a solubility of at least 30 grams per 100 grams of water.
[8]
8. Method, according to claim 1, CHARACTERIZED by the fact that the temperature of the solution is decreased by a gradient cooling method with a temperature change rate of about 1 ° C per minute to am

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法律状态:
2018-02-14| B06F| Objections, documents and/or translations needed after an examination request according art. 34 industrial property law|

2018-03-27| B15K| Others concerning applications: alteration of classification|Ipc: A23L 27/30 (2016.01), A23G 3/36 (2006.01), A23G 9/ |

2018-09-11| B07A| Technical examination (opinion): publication of technical examination (opinion)|

2019-08-20| B09A| Decision: intention to grant|

2019-10-29| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 10/02/2012, OBSERVADAS AS CONDICOES LEGAIS. (CO) 20 (VINTE) ANOS CONTADOS A PARTIR DE 10/02/2012, OBSERVADAS AS CONDICOES LEGAIS |

优先权:

申请号 | 申请日 | 专利标题

US201161441443P| true| 2011-02-10|2011-02-10|

PCT/US2012/024585|WO2012109506A1|2011-02-10|2012-02-10|Highly soluble stevia sweetener|

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