Methods of separating a corn fiber lipid fraction from corn fiber

• US 6,589,760 B1
• Filed: 02/10/2000
• Issued: 07/08/2003
• Est. Priority Date: 02/10/1999
• Status: Expired due to Fees

• Current Assignee: Eastman Chemical Company
• Original Assignee: Eastman Chemical Company
• Inventors: Wood, Matthew D., Debenham, John S., Buchanan, Norma L., Shelton, Michael C., Buchanan, Charles M.
• Primary Examiner(s): GITOMER, RALPH J
• Application Number:
  US09/501,917
• Time in Patent Office: 1,244 Days
• Field of Search: 435/23, 424/750, 552/545
• US Class Current: 435/23
• CPC Class Codes: A23D 9/007 characterised by ingredients other than fatty acid triglycerides
• CPC Class Codes: A23D 9/02 characterised by the production or working-up
• CPC Class Codes: A23K 10/37 from waste material from hydrolysates of wood or straw A23K10/32; from molasses A23K10/33
• CPC Class Codes: A23K 20/147 Polymeric derivatives, e.g. peptides or proteins
• CPC Class Codes: A23K 20/163 Sugars; Polysaccharides
• CPC Class Codes: A23L 29/262 Cellulose; Derivatives thereof, e.g. ethers
• CPC Class Codes: A23L 33/11 Plant sterols or derivatives thereof, e.g. phytosterols
• CPC Class Codes: A23L 33/115 Fatty acids or derivatives thereof; Fats or oils
• CPC Class Codes: A23L 33/24 Cellulose or derivatives thereof
• CPC Class Codes: A23L 7/107 Addition or treatment with enzymes not combined with fermentation with microorganisms
• CPC Class Codes: A23L 7/115 Cereal fibre products, e.g. bran, husk
• CPC Class Codes: A23V 2002/00 Food compositions, function of food ingredients or processes for food or foodstuffs
• CPC Class Codes: A23V 2250/602 Arabinose
• CPC Class Codes: A23V 2250/626 Ribose
• CPC Class Codes: A23V 2250/638 Xylose
• CPC Class Codes: C08B 11/00 Preparation of cellulose ethers rendering cellulose suitable for etherification C08B1/06
• CPC Class Codes: C08B 3/00 Preparation of cellulose esters of organic acids rendering cellulose suitable for esterification C08B1/02
• CPC Class Codes: C08B 30/10 Working-up residues from the starch extraction , e.g. potato peel or steeping water, including pressing water from the starch-extracted material
• CPC Class Codes: C08B 37/0057 beta-D-Xylans, i.e. xylosaccharide, e.g. arabinoxylan, arabinofuronan, pentosans; (beta-1,3)(beta-1,4)-D-Xylans, e.g. rhodymenans; Hemicellulose; Derivatives thereof
• CPC Class Codes: C08B 37/006 Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
• CPC Class Codes: C11B 1/025 : by enzymes or microorganisms, living or dead
• CPC Class Codes: C11B 1/10 : by extracting
• CPC Class Codes: C13K 1/02 : obtained by saccharification of cellulosic materials manufacture of fodder A23K10/32
• CPC Class Codes: C13K 1/08 : Purifying
• CPC Class Codes: C13K 13/00 : Sugars not otherwise provided for in this class
• CPC Class Codes: C13K 13/002 : Xylose
• CPC Class Codes: D21C 5/00 : Other processes for obtaining cellulose, e.g. cooking cotton linters obtaining fibres for spinning D01C; Processes characterised by the choice of cellulose-containing starting materials
• CPC Class Codes: D21C 5/005 : Treatment of cellulose-containing material with microorganisms or enzymes
• CPC Class Codes: Y02P 60/87 : Re-use of by-products of food processing for fodder production
• CPC Class Codes: Y02W 30/74 : Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

Abstract

The invention provides a method of separating from corn fiber a lipid fraction having phytosterol esters and phytosterols where the method has the steps of: (a) heating an aqueous mixture of unground corn fiber; (b) contacting the mixture of step (a) with at least one enzyme suitable for digesting starch for a time and at a temperature suitable to provide a mixture of an essentially destarched corn fiber and a liquid comprising soluble carbohydrates; (c) contacting the mixture of step (a) or (b) with a protease enzyme to provide a proteolyzed corn fiber and a liquid; (d) separating the liquid of step (c) from the corn fiber to provide a destarched, proteolyzed corn fiber; and (e) extracting the destarched, proteolyzed corn fiber with at least one organic solvent. A corn fiber lipid fraction/organic solvent solution having phytosterol esters and phytosterols is provided. The invention also provides a corn fiber lipid fraction containing phytosterols and phytosterol esters obtained via solvent extraction of a proteolyzed corn fiber. The concentration of phytosterols and phytosterol esters in the lipid fraction is at least about 1.4 times greater than the concentration of phytosterols and phytosterol esters in the lipid fraction of a nonproteolyzed corn fiber.

Claims

1. A method of separating a corn fiber lipid fraction having phytosterol esters and phytosterols wherein the method comprises the steps of:

a. providing a mixture of corn fiber and water;

b. contacting the mixture with an amylase enzyme and a protease enzyme to provide a destarched and proteolyzed corn fiber and a liquid;

c. separating the liquid from the destarched and proteolyzed corn fiber; and

d. extracting the destarched and proteolyzed corn fiber with at least one organic solvent,

thereby providing a corn fiber lipid fraction/organic solvent solution having phytosterol esters and phytosterols, wherein the concentration of phytosterols in the lipid fraction is at least about 1.4 times greater than the concentration of phytosterols in the lipid fraction extracted from a nondestarched and nonproteolyzed corn fiber.

2. The method of claim 1, wherein the corn fiber is unground.

3. The method of claim 1, further comprising conducting a corn fiber grinding step prior to step (a).

4. The method of claim 1, wherein the corn fiber is destarched with an amylase enzyme prior to or concurrently with the protease enzyme contacting step.

5. The method of claim 4, wherein the amylase enzyme contacting step is conducted at a temperature of from about 25°

C. to about 120°

C. for about 0.1 h to about 24 h at a pH of from about 4 to about 9.

6. The method of claim 4, wherein the amylase enzyme contacting step is conducted at a temperature of from about 60°

C. to about 90°

C. for about 1 h to about 12 h at a pH of from about 7 to about 9.

7. The method of claim 1, wherein the protease enzyme contacting step is conducted at a temperature of from about 25°

C. to about 120°

C. for from about 0.1 h to about 24 h at a pH of from about 4 to about 9.

8. The method of claim 1, wherein the protease enzyme contacting step is conducted at a temperature of from about 60°

C. to about 90°

C. for from about 1 h to about 12 h at a pH of from about 7 to about 9.

9. The method of claim 1, wherein the corn fiber contacted with protease enzyme is not dried prior to the solvent extraction step.

10. The method of claim 1, wherein the corn fiber contacted with protease enzyme is dried prior to the solvent extraction step.

11. The method of claim 1, wherein the solvent is a polar organic solvent.

12. The method of claim 11, wherein the organic solvent comprises methanol, ethanol, isopropyl alcohol, n-butyl alcohol, acetone, ethyl acetate, methyl isobutyl ketone, methyl ethyl ketone, or a mixture thereof.

13. The method of claim 1, wherein the organic solvent comprises hexane, heptane, diethyl ether, or a mixture thereof.

14. The method of claim 1, wherein the solvent extraction step is conducted at a temperature of from about 0°

C. to about 115°

C. for from about 1 min to about 600 min.

15. The method of claim 1, wherein the solvent extraction step is conducted at a temperature of from about 20°

C. to about 80°

C. for from about 10 to about 60 min.

16. The method of claim 1, further comprising separating the corn fiber lipid fraction from the organic solvent solution via a distillation step wherein the phytosterols and phytosterol esters are separated with the corn fiber lipid fraction.

17. The method of claim 16, wherein prior to conducting the distillation step a water layer is separated from the corn fiber lipid fraction/organic solvent solution.

18. The method of claim 16, wherein after conducting the distillation step a water layer is separated from the corn fiber lipid fraction/organic solvent solution.

19. The method of claim 16, wherein the organic solvent solution is separated from the corn fiber lipid fraction via vacuum distillation.

20. The method of claim 19, wherein the corn fiber lipid fraction is enriched in phytosterols and phytosterol esters.

21. The method of claim 16, further comprising separating the phytosterol esters and phytosterols from the corn fiber lipid fraction and, optionally, separating the phytosterols and phytosterol esters from each other.

22. The method of claim 21, further comprising separating the phytosterol esters and phytosterols from the corn fiber lipid fraction and, optionally, from each other, wherein the separation is conducted via crystallization.

23. The method of claim 16, wherein unwanted components are present in the corn fiber lipid fraction with the phytosterols and phytosterol esters and wherein the method further comprises the steps of:

separating the unwanted components from the corn fiber lipid fraction via extraction to provide a corn fiber lipid fraction enriched in phytosterol esters and phytosterols; and

separating the phytosterol esters and phytosterols from the lipid fraction and, optionally, separating the phytosterols and phytosterol esters from each other, wherein the separation is conducted via crystallization.

24. The method of claim 16, wherein glyceride esters are present in the corn fiber lipid fraction with the phytosterols and phytosterol esters and wherein the method further comprises the steps of:

hydrolyzing the glyceride esters;

removing the hydrolyzed glyceride esters to provide a corn fiber lipid fraction enriched in phytosterol esters and phytosterols; and

separating the phytosterol esters and phytosterols from the lipid fraction and, optionally, separating the phytosterols and phytosterol esters from each other, wherein the separation is conducted via crystallization.