Granted Patent B2

US 7,923,552 · App. 11/252,430 · Granted Apr 12, 2011

Assignee: SGF Holdings, LLC

Abstract

Claims (88)

1. A method of purifying rebaudioside A from Stevia starting material comprising: (i) formulating a selected EtOH solvent consisting of water and ethanol, (ii) performing a first reflux stage by refluxing the Stevia starting material in the selected EtOH solvent and optionally performing additional reflux stages using retentate isolated from a refluxed mixture or from a stirred wash mixture, (iii) optionally, performing one or more stirred wash stages, and (iv) performing an ethanol purge and drying stage,

wherein formulating a selected EtOH solvent comprises either (A) a reflux solvent approximation, wherein, based on the asserted or labeled purity of a batch of Stevia starting material, for a Stevia starting material labeled or asserted to be 90% rebaudioside A purity, the reflux solvent is formulated as ethanol and water, and for every 5% decrease in rebaudioside A purity below 90% rebaudioside A purity in the Stevia starting material, based on the asserted or labeled purity of a batch of Stevia starting material, increasing the water content of reflux solvent 1% above a baseline of 6% water, and the remaining volume of the reflux solvent is ethanol, or (B) preparing a series of test mixtures in which the water content is uniformly incremented from 0.5% to 15%, or within a subset of that 0.5% to 15% range, and the balance of solvent in each such test mixture is ethanol, assaying the retentate of a reflux of the Stevia starting material in each test mixture for rebaudioside A purity, and selecting as the selected EtOH solvent the test mixture that produces a retentate with the highest purity rebaudioside A.

2. A method of purifying rebaudioside A from Stevia starting material comprising:

Formulating a selected EtOH solvent consisting of water and ethanol for the Stevia starting material;

Mixing and refluxing the Stevia starting material in the selected EtOH solvent to create a refluxed mixture;

Separating a retentate by filtering the refluxed mixture;

Mixing and stirring the retentate in ethanol to create a stirred wash mixture;

Separating a retentate by filtering the stirred wash mixture; and

Purging the ethanol and drying the retentate, wherein the dried retentate is rebaudioside A,

wherein formulating a selected EtOH solvent for the Stevia starting material comprises either (A) a reflux solvent approximation, wherein, based on the asserted or labeled purity of a batch of Stevia starting material, for a Stevia starting material labeled or asserted to be 90% rebaudioside A purity, the reflux solvent is formulated as ethanol and water, and for every 5% decrease in rebaudioside A purity below 90% rebaudioside A purity in the Stevia starting material, based on the asserted or labeled purity of a batch of Stevia starting material, increasing the water content of reflux solvent 1% above a baseline of 6% water, and the remaining volume of the reflux solvent is ethanol, or (B) preparing a series of test mixtures in which the water content is uniformly incremented from 0.5% to 15%, or within a subset of that 0.5% to 15% range, and the balance of solvent in each such test mixture is ethanol, assaying the retentate of a reflux of the Stevia starting material in each test mixture for rebaudioside A purity, and selecting as the selected EtOH solvent the test mixture that produces a retentate with the highest purity rebaudioside A.

3. A method of purifying rebaudioside A from Stevia starting material comprising:

Formulating a selected EtOH solvent consisting of water and ethanol for the Stevia starting material;

Mixing and refluxing the Stevia starting material in the selected EtOH solvent to create a refluxed mixture;

Separating a retentate by filtering the refluxed mixture, and optionally mixing and stirring the retentate in ethanol to create a stirred wash mixture and separating a retentate by filtering the stirred wash mixture;

Mixing and refluxing the retentate in the selected EtOH solvent to create a refluxed mixture;

Separating a retentate by filtering the refluxed mixture, and optionally mixing and stirring the retentate in ethanol to create a stirred wash mixture and separating a retentate by filtering the stirred wash mixture;

Optionally repeating one or more times the preceding two steps; and

Purging the ethanol and drying the retentate, wherein the dried retentate is rebaudioside A,

wherein formulating a selected EtOH solvent for the Stevia starting material comprises either (A) a reflux solvent approximation, wherein, based on the asserted or labeled purity of a batch of Stevia starting material, for a Stevia starting material labeled or asserted to be 90% rebaudioside A purity, the reflux solvent is formulated as ethanol and water, and for every 5% decrease in rebaudioside A purity below 90% rebaudioside A purity in the Stevia starting material, based on the asserted or labeled purity of a batch of Stevia starting material, increasing the water content of reflux solvent 1% above a baseline of 6% water, and the remaining volume of the reflux solvent is ethanol, or (B) preparing a series of test mixtures in which the water content is uniformly incremented from 0.5% to 15%, or within a subset of that 0.5% to 15% range, and the balance of solvent in each such test mixture is ethanol, assaying the retentate of a reflux of the Stevia starting material in each test mixture for rebaudioside A purity, and selecting as the selected EtOH solvent the test mixture that produces a retentate with the highest purity rebaudioside A.

4. The method of claim 1 , 2 , or 3 , wherein the method of mixing and refluxing the Stevia starting material comprises:

Mixing 1 part by mass of Stevia starting material with from 3 to 10 parts by volume, more preferably from 4 to 6 parts by volume, and most preferably approximately 4 parts by volume of the selected EtOH solvent to create a reflux mixture; and

Refluxing the reflux mixture in an appropriate apparatus at approximately the boiling point of ethanol for approximately one hour.

5. The method of claim 1 or 3 , wherein the method of mixing and refluxing the retentate in one or more additional refluxes comprises:

Mixing 1 part by mass of the retentate with from 3 to 10 parts by volume, more preferably from 4 to 6 parts by volume, and most preferably approximately 4 parts by volume of the selected EtOH solvent to create a reflux mixture; and

Refluxing the reflux mixture in an appropriate apparatus at approximately the boiling point of ethanol for approximately one hour.

6. The method of claim 1 , 2 , or 3 , wherein the method of separating retentate by filtering the refluxed mixture or stirred wash mixture comprises:

Filtering the mixture using a filtering means appropriate for the volume of refluxed mixture and throughput required and that separates particles with an axis or diameter approximately greater than 2.0 μm, more preferably greater than 1.5 μm; and most preferably equal to or greater than 0.1 μm; and

Collecting the separated particles from the filtering means.

7. The method of claim 1 , 2 , or 3 , wherein the method of mixing and stirring in a stirred wash retentate from a previous step and separating retentate by filtering the stirred wash mixture comprises:

Mixing 1 part by mass of the isolated rebaudioside A with from 3 to 10 parts by volume, more preferably from 4 to 6 parts by volume, and most preferably approximately 4 parts by volume of ethanol to create a wash mixture;

Stirring the wash mixture in an appropriate apparatus for approximately fifteen minutes;

Filtering the wash mixture using a filtering means appropriate for the volume of refluxed mixture and throughput required and that separates particles with an axis or diameter approximately greater than 2.0 μm, more preferably greater than 1.5 μm; and most preferably equal to or greater than 0.1 μm; and

Collecting the separated particles from the filtering means.

8. The method of claim 1 , 2 , or 3 , wherein the method of purging the ethanol and drying the isolated rebaudioside A comprises, in a laboratory embodiment of the invention, drying the isolated rebaudioside A is an oven, preferably a blower oven, at or above 79° C., and, in an industrial embodiment, of the invention:

Mixing 1 part by mass of retentate, isolated in a preceding step by filtering a refluxed mixture or a stirred wash mixture, with water such that the ultimate mixture volume is approximately twice the mass of the retentate;

Heating the mixture in a vented vessel to at least 79° C. while stirring;

Stirring the mixture until the ethanol content of the mixture is equal to or less than the maximum ethanol content permitted by an associated spray dryer;

Feeding the mixture to the spray dryer; and

Collecting the dried rebaudioside A.

9. The method of claim 1 , 2 , or 3 , wherein ethanol used in formulating the EtOH solvent and in the selected EtOH solvent is either absolute ethanol or denatured ethanol.

10. The method of claim 1 , 2 , or 3 , wherein an alkanol other than ethanol is used in place of ethanol in the selected EtOH solvent.

11. The method of claim 1 , 2 , or 3 , wherein an alkanol is used in place of ethanol in the selected EtOH solvent and in any stirred wash stages.

12. The method of claim 1 , 2 , or 3 , wherein a first alkanol is used in the selected EtOH solvent, and a second alkanol is used in any stirred wash stages.

13. The method of claim 1 , 2 , or 3 , wherein the method of formulating the selected EtOH solvent includes a mass to volume ratio assay.

14. A method of purifying rebaudioside A from Stevia starting material comprising: (i) formulating a selected EtOH solvent consisting of water and ethanol, (ii) performing a first reflux stage by refluxing the Stevia starting material in the selected EtOH solvent and optionally performing additional reflux stages using retentate isolated from a refluxed mixture or from a stirred wash mixture, (iii) optionally, performing one or more stirred wash stages, and (iv) performing an ethanol purge and drying stage,

wherein formulating a selected EtOH solvent comprises preparing a series of test mixtures in which the water content is uniformly incremented from 0.5% to 15%, or within a subset of that 0.5% to 15% range, and the balance of solvent in each such test mixture is ethanol, assaying the retentate of a reflux of the Stevia starting material in each test mixture for rebaudioside A purity and yield, and selecting as the selected EtOH solvent the test mixture that produces a retentate with the highest yield of rebaudioside A final product that has a rebaudioside A purity acceptable to the user.

15. A method of purifying rebaudioside A from Stevia starting material comprising:

Formulating a selected EtOH solvent consisting of water and ethanol for the Stevia starting material;

Mixing and refluxing the Stevia starting material in the selected EtOH solvent to create a refluxed mixture;

Separating a retentate by filtering the refluxed mixture;

Mixing and stirring the retentate in ethanol to create a stirred wash mixture;

Separating a retentate by filtering the stirred wash mixture; and

Purging the ethanol and drying the retentate, wherein the dried retentate is rebaudioside A,

wherein formulating a selected EtOH solvent for the Stevia starting material comprises preparing a series of test mixtures in which the water content is uniformly incremented from 0.5% to 15%, or within a subset of that 0.5% to 15% range, and the balance of solvent in each such test mixture is ethanol, assaying the retentate of a reflux of the Stevia starting material in each test mixture for rebaudioside A purity and yield, and selecting as the selected EtOH solvent the test mixture that produces a retentate with the highest yield of rebaudioside A final product that has a rebaudioside A purity acceptable to the user.

16. A method of purifying rebaudioside A from Stevia starting material comprising:

Formulating a selected EtOH solvent consisting of water and ethanol for the Stevia starting material;

Mixing and refluxing the Stevia starting material in the selected EtOH solvent to create a refluxed mixture;

Separating a retentate by filtering the refluxed mixture, and optionally mixing and stirring the retentate in ethanol to create a stirred wash mixture and separating a retentate by filtering the stirred wash mixture;

Mixing and refluxing the retentate in the selected EtOH solvent to create a refluxed mixture;

Separating a retentate by filtering the refluxed mixture, and optionally mixing and stirring the retentate in ethanol to create a stirred wash mixture and separating a retentate by filtering the stirred wash mixture;

Optionally repeating one or more times the preceding two steps; and

Purging the ethanol and drying the retentate, wherein the dried retentate is rebaudioside A,

wherein formulating a selected EtOH solvent for the Stevia starting material comprises preparing a series of test mixtures in which the water content is uniformly incremented from 0.5% to 15%, or within a subset of that 0.5% to 15% range, and the balance of solvent in each such test mixture is ethanol, assaying the retentate of a reflux of the Stevia starting material in each test mixture for rebaudioside A purity and yield, and selecting as the selected EtOH solvent the test mixture that produces a retentate with the highest yield of rebaudioside A final product that has a rebaudioside A purity acceptable to the user.

17. The method of claim 14 , 15 , or 16 , wherein the method of formulating the selected EtOH solvent includes a mass to volume ratio assay.

18. The method of claim 14 , 15 , or 16 , wherein the method of mixing and refluxing the Stevia starting material comprises:

Mixing 1 part by mass of Stevia starting material with from 3 to 10 parts by volume of the selected EtOH solvent to create a reflux mixture; and

Refluxing the reflux mixture in an appropriate apparatus at approximately the boiling point of ethanol for approximately one hour.

19. The method of claim 14 or 16 , wherein the method of mixing and refluxing the retentate in one or more additional refluxes comprises:

Mixing 1 part by mass of the retentate with from 3 to 10 parts by volume of the selected EtOH solvent to create a reflux mixture; and

Refluxing the reflux mixture in an appropriate apparatus at approximately the boiling point of ethanol for approximately one hour.

20. The method of claim 14 , 15 , or 16 , wherein the method of separating retentate by filtering the refluxed mixture or stirred wash mixture comprises:

Filtering the mixture using a filtering means appropriate for the volume of refluxed mixture and throughput required and that separates particles with an axis or diameter approximately equal to or greater than 0.1 μm; and

Collecting the separated particles from the filtering means.

21. The method of claim 14 , 15 , or 16 , wherein the method of mixing and stirring in a stirred wash retentate from a previous step and separating retentate by filtering the stirred wash mixture comprises:

Mixing 1 part by mass of the isolated rebaudioside A with from 3 to 10 parts by volume of ethanol to create a wash mixture;

Stirring the wash mixture in an appropriate apparatus for approximately fifteen minutes;

Filtering the wash mixture using a filtering means appropriate for the volume of refluxed mixture and throughput required and that separates particles with an axis or diameter approximately equal to or greater than 0.1 μm; and

Collecting the separated particles from the filtering means.

22. The method of claim 14 , 15 , or 16 , wherein the method of purging the ethanol and drying the isolated rebaudioside A comprises, in a laboratory embodiment of the invention, drying the isolated rebaudioside A is an oven, preferably a blower oven, at or above 79° C., and, in an industrial embodiment, of the invention:

Mixing 1 part by mass of retentate, isolated in a preceding step by filtering a refluxed mixture or a stirred wash mixture, with water such that the ultimate mixture volume is approximately twice the mass of the retentate;

Heating the mixture in a vented vessel to at least 79° C. while stirring;

Stirring the mixture until the ethanol content of the mixture is equal to or less than the maximum ethanol content permitted by an associated spray dryer;

Feeding the mixture to the spray dryer; and

Collecting the dried rebaudioside A.

23. The method of claim 14 , 15 , or 16 , wherein ethanol used in formulating the EtOH solvent and in the selected EtOH solvent is either absolute ethanol or denatured ethanol.

24. The method of claim 14 , 15 , or 16 , wherein an alkanol other than ethanol is used in place of ethanol in the selected EtOH solvent.

25. The method of claim 14 , 15 , or 16 , wherein an alkanol is used in place of ethanol in the selected EtOH solvent and in any stirred wash stages.

26. The method of claim 14 , 15 , or 16 , wherein a first alkanol is used in the selected EtOH solvent, and a second alkanol is used in any stirred wash stages.

Assignments (12)

Continuity (3)