Process for the purification of marigold xanthophylls

• US 7,150,890 B2
• Filed: 09/22/2004
• Issued: 12/19/2006
• Est. Priority Date: 09/22/2003
• Status: Expired due to Fees

• Current Assignee: Alfonso, Mr. Poblete Vidal
• Original Assignee: Alfonso, Mr. Poblete Vidal
• Inventors: Cardona, M. C. Mario D. Torres, Rosales, Jose Antonio Socla
• Primary Examiner(s): TATE, CHRISTOPHER ROBIN
• Application Number:
  US10/948,088
• Publication Number:
  US 20050153002A1
• Time in Patent Office: 818 Days
• Field of Search: None
• US Class Current: 424/778
• CPC Class Codes: A61K 36/064 Saccharomycetales, e.g. baker's yeast
• CPC Class Codes: A61K 36/28 Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
• CPC Class Codes: C12P 23/00 Preparation of compounds containing a cyclohexene ring having an unsaturated side chain containing at least ten carbon atoms bound by conjugated double bonds, e.g. carotenes containing heterorings C12P17/00

Abstract

Description of a process to extract, saponify and purify lutein and zeaxantine contained in Marigold flowers free from any genetic manipulation, which have been harvested by hand and dried upon weather so that it neither contains epoxicarotenoids or cis-carotenoids. Fatty acids are removed as its metallic salts and carotenoids are recovered using a polar solvent.

Claims

1. A process for obtaining xanthophylls from marigold petals, the process comprising:

drying harvested marigold petals at a predetermined temperature range for a predetermined time period to produce dried petals;

saponifying the dried petals to obtain saponified extracts;

dissolving the saponified extracts in water to produce a mixture including emulsions containing from 1 to 20 grams of carotenoids per kilogram of the mixture;

adding at least one metallic halide to the mixture to adjust a pH of the mixture such that the pH is between about 1 and about 6;

filtering the pH-adjusted mixture to remove substantially all liquid from the mixture to produce a resultant solid; and

washing the resultant solid with a polar solvent to recover desired xanthophylls.

2. The process of claim 1, further comprising:

harvesting marigold petals from marigold flowers that are free of any genetic manipulations to produce the harvested marigold petals.

3. The process of claim 2, wherein the marigold flowers have been cultivated without using a pesticide.

4. The process of claim 1, wherein the step of drying harvested marigold petals comprises:

drying harvested marigold petals at a temperature range between about 20°

C. and about 45°

C.

5. The process of claim 1, wherein the step of drying harvested marigold petals comprises:

drying harvested marigold petals for a time period of about one week to about four weeks under predetermined environmental conditions.

6. The process of claim 1, further comprising:

adding a solution containing 0.005 to 0.100% by weight of hydrolytic enzymes to the harvested marigold petals prior to the step of drying.

7. The process of claim 6, wherein the hydrolytic enzymes include at least one of cellulase, pectinase, lipase, and protease.

8. The process of claim 1, wherein the polar solvent comprises at least one of saturated hydrocarbon of short chain C5–

C8, halogenated hydrocarbon, pentane, hexane, heptane, and octane.

9. The process of claim 1, wherein the polar solvent comprises at least one of methylene chloride, chloroform, carbon tetrachloride, and dichloroethylene.

10. The process of claim 1, wherein the step of dissolving comprises:

dissolving the saponified extracts in water to produce a mixture including emulsions containing from 5 to 15 grams of xanthophylls.

11. The process of claim 1, wherein fatty acids of the mixture react with the metallic halide.

12. The process of claim 1, wherein the metallic halide comprises at least one of calcium chloride, magnesium chloride, and zinc chloride.

13. The process of claim 1, wherein the step of adding at least one metallic halide to the mixture comprises adding at least one metallic halide to the mixture to adjust a pH of the mixture such that the pH is between about 3 and about 5.

14. The process of claim 1, wherein the polar solvent comprises an alcohol.

15. The process of claim 1, wherein the polar solvent comprises an acetone.

16. The process of claim 1, wherein the step of washing the resultant solid comprises:

washing the resultant solid at a temperature between about 20°

C. and about 45°

C.

17. The process of claim 1, wherein the step of saponifying the dried petals comprises:

saponifying the dried petals to obtain saponified extracts such that the saponified extracts are free of epoxicarotenoids.

18. The process of claim 1, wherein the step of washing the resultant solid comprises:

washing the resultant solid with a polar solvent to produce desired xanthophylls that are substantially free of cis-carotenoids.

19. The process of claim 1, wherein the step of washing the resultant solid comprises:

washing the resultant solid with a polar solvent to produce desired xanthophylls that are substantially free of epoxicarotenoids.

20. The process of claim 1, wherein the saponified extracts contain from about 80 to about 250 grams of carotenoids per kilogram of which about 90% to about 95% of the carotenoids is lutein and of which about 5% to about 10% of the carotenoids is zeaxanthin.

21. The process of claim 1, wherein the step of washing the resultant solid comprises:

washing the resultant solid with a polar solvent to produce a concentrate of xanthophylls containing about 900 grams of xanthophylls per kilogram of which about 95% is lutein and about 5% is zeaxanthin.

22. The process of claim 1, wherein the desired pigments comprise a concentrated product of lutein and zeaxanthin that is appropriate for human consumption.

23. The process of claim 1, further comprising:

evaporating the polar solvent to produce a concentrate of lutein and zeaxanthin that is free of the polar solvent.