Method and system for production of zein and/or xanthophylls using chromatography

• US 8,236,929 B2
• Filed: 05/08/2007
• Issued: 08/07/2012
• Est. Priority Date: 05/08/2006
• Status: Active Grant

• Current Assignee: Board of Trustees of The University of Illinois
• Original Assignee: Board of Trustees of The University of Illinois
• Inventors: Cheryan, Munir, Kale, Aniket V., Zhu, Fangyi, Shane, Philip L.
• Primary Examiner(s): DESAI, ANAND U
• Application Number:
  US11/990,471
• Publication Number:
  US 20090215990A1
• Time in Patent Office: 1,918 Days
• Field of Search: None
• US Class Current: 530/373
• CPC Class Codes: C07K 14/415 from plants
• CPC Class Codes: C09B 61/00 Dyes of natural origin prepared from natural sources , e.g. vegetable sources
• CPC Class Codes: Y02E 50/10 Biofuels, e.g. bio-diesel

Abstract

Methods and systems for obtaining zein and/or xanthophylls in highly pure form. Zein is first extracted from corn using aqueous ethanol. Suspended corn solids are separated, and the resulting extract is purified in a single size-exclusion chromatography step to separate impurities and produce substantially purified zein. The chromatography step may simultaneously produce substantially purified xanthophylls.

Claims

1. A process for producing zein and xanthophylls from corn, the process comprising:

extracting soluble compounds from a corn-based material with wan alcohol solvent to provide a corn-solvent mixture, the soluble compounds comprising at least zein and xanthophylls;

first separation of the corn-solvent mixture into two streams, of which one stream is an extract containing substantially the zein, impurities, xanthophylls and solvent, wherein the impurities comprise substantially all components in the extract other than solvent, zein and xanthophylls, and another stream containing the remaining corn solids and solvent, said first separation comprising at least one of centrifugation, filtration, and membrane microfiltration;

second separation of a zein fraction and a xanthophylls fraction from the extract containing substantially the zein, impurities, xanthophylls and solvent to provide an eluted zein fraction and an eluted xanthophyll fraction, said second separation comprising chromatography based on a size-exclusion mechanism;

concentrating the separated zein fraction eluted from said second separation by removing the solvent; and

concentrating the separated xanthophylls fraction eluted from said second separation by removing the solvent.

2. The process of claim 1,

wherein said second separation separates the separated zein fraction and the separated xanthophylls fraction in a single step.

3. The process of claim 2, wherein said concentrating the separate zein comprises nanofiltration.

4. The process of claim 2, wherein said concentrating the separate zein comprises using reverse osmosis.

5. The process of claim 2, wherein said concentrating the separated zein comprises using adsorption chromatography.

6. The process of claim 5, wherein a mobile phase used for elution in the adsorption chromatography comprises ethyl acetate.

7. The process of claim 1, further comprising:

before said second separation, concentrating the extract to provide a higher level of solids in a concentrated extract, wherein said concentrating comprises membrane filtration;

wherein said second separation separates said concentrated extract.

8. The process of claim 7, wherein said concentrating the extract further comprises dehydration.

9. The process of claim 1, further comprising:

before said second separation, concentrating the extract to provide a higher level of solids in a concentrated extract, wherein said concentrating comprises membrane filtration, wherein said second separation separates said concentrated extract.

10. The process of claim 1, wherein the alcohol is aqueous ethanol.

11. The process of claim 10, wherein the alcohol is aqueous ethanol including a mixture of 60-100% ethanol by volume and water.

12. The process of claim 1, wherein said extraction comprises at least one of batch and continuous extraction.

13. The process of claim 1, wherein said first separation comprises centrifugation.

14. The process of claim 1, wherein said first separation comprises filtration.

15. The process of claim 1, wherein said first separation comprises membrane microfiltration.

16. The process of claim 1, wherein chromatographic media used in said second separation has a molecular weight exclusion limit of 10,000 or less.

17. The process of claim 16 wherein the chromatographic media has a molecular weight exclusion limit of 5000 or less.

18. The process of claim 1, wherein the solvent is aqueous ethanol, and wherein a mobile phase used in said second separation to elute the fractions comprises aqueous alcohol.

19. The process of claim 1, further comprising:

fractionating the impurities after said second separation.

20. The process of claim 1, wherein the corn-based material comprises at least one of corn gluten meal, distillers dried grains with or without solubles, and corn-based materials that have been partially or substantially de-oiled.

21. The process of claim 1, wherein the separated zein has a purity of at least 90%.

26. The process of claim 1, wherein the corn comprises whole ground corn.

28. The process of claim 1, wherein said second separation occurs directly from the extract resulting from said first separation.

22. A process for producing zein and xanthophyll from corn, the process comprising:

extraction of soluble compounds from a corn-based material with an aqueous ethanol solvent to provide a corn-solvent mixture, the soluble compounds comprising at least zein and/or xanthophylls;

first separation of the corn-solvent mixture into two streams, of which one stream is an extract containing substantially the zein, xanthophylls, impurities, and solvent, and another stream containing the remaining corn solids and solvent, said first separation comprising at least one of centrifugation, filtration, and membrane microfiltration, wherein the impurities comprise substantially all components in the extract other than solvent, zein, and xanthophylls;

second separation of a zein fraction and a xanthophylls fraction from the extract comprising the impurities in a single step, said second separation comprising chromatography based on a size-exclusion mechanism, wherein said second separation uses a mobile phase comprising aqueous ethanol;

concentrating the separated zein fraction eluting from the column by removing the solvent;

concentrating the separated xanthophyll fraction eluting from the column by removing the solvent; and

recycling the aqueous ethanol from the mobile phase.

23. The process of claim 22, wherein the aqueous ethanol in both said extraction and said second separation have substantially the same ethanol concentration.

24. The process of claim 22, wherein the aqueous ethanol in both said extraction and said second separation have an ethanol concentration of about 70-95%.

25. The process of claim 22, further comprising:

recycling ethanol from at least one of said extraction, said first separation, said concentrating the separated zein fraction, and said concentrating the separated xanthophyll fraction.

27. The process of claim 22, wherein the corn comprises whole ground corn.