Process for the preparation of high purity phytosterols from deodourizer distillate from vegetable oils

• US 20070142652A1
• Filed: 03/13/2006
• Published: 06/21/2007
• Est. Priority Date: 11/08/2005
• Status: Active Grant

• Current Assignee: Council of Scientific & Industrial Research
• Original Assignee: Council of Scientific & Industrial Research
• Inventors: Sobankumar, Das, Arumughan, Chami, Rajam, Leelavathy, Sudaresan, Andikkannu, Yohesh, Kannan, Nair, Sreeja
• Granted Patent: US 7,632,530 B2
• Time in Patent Office: Days
• US Class Current: 552/540
• CPC Class Codes: A23V 2002/00 Food compositions, function of food ingredients or processes for food or foodstuffs
• CPC Class Codes: A23V 2250/21364 Campesterol
• CPC Class Codes: A23V 2250/21372 Sitosterol
• CPC Class Codes: A23V 2250/21376 Stigmasterol
• CPC Class Codes: C07J 9/00 Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
• CPC Class Codes: C11B 13/00 Recovery of fats, fatty oils or fatty acids from waste materials
• CPC Class Codes: Y02W 30/74 Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

Abstract

The present invention provides an isolation process of the pure sterols from the SODD by simple acid catalyzed esterification and the separation of the reagents by distillation and water washing followed by the crystallization of phytosterols and purification. Soybean oil deodorizer distillate (SODD) and distillate from other vegetable oil refining contain free sterols, in addition to steryl esters, tocopherols squalene and unknown compounds. The process is also applicable to other vegetable oil distillate containing more than 1% phytosterols in the free form. Phytosterols thus obtained is of high purity (95-99%) and high yield (80-90%) and contains β-sitosterol, Stigmasterol and campesterol.

Claims

1. A process for the preparation of high purity phytosterols from deodourizer distillate from vegetable oils which comprises mixing deodourizer distillate from vegetable oils with a methanolic solution of sulfuric acid in a ratio of 1:

1 to 1;

1.5 (v/v), stirring the above said reaction mixture, at a temperature of 50-85°

C., for a period of 2-4 hrs, distilling of the excess of methanol from the above said reaction mixture under vacuum, adding brine solution to the above said reaction mixture to separate sulfuric acid and removing the lower layer to obtain the ester layer, washing the above said ester layer with hot water till all of the acid and salts are removed, followed by crystallization at a temperature in the range of 0-25°

C. for a period of 110 hrs, filtering and washing the resultant crystals obtained with chilled n-hexane, at a temperature of 0-10°

C. to obtain the desired high purity phytosterols.

2. A process as claimed in claim 1, wherein the vegetable oil used for obtaining deodourizer distillate is selected from the group consisting of soybean oil, sunflower oil, rice bran oil, palm kernel oil and coconut oil.

3. A process as claimed in claim 1, wherein the sulfuric acid in methanolic solution of sulfuric acid used is in the range of 1-10%.

4. A process as claimed in claim 1, wherein the crystallization of the sterols is facilitated by bound water retained after water washing or added externally.

5. A process as claimed in claim 1, wherein the excess water present in the ester layer is released by controlled heating and is removed by decantation or centrifugation.

6. A process as claimed in claim 1, wherein the yield of fatty acid methyl esters obtained is 60-70% of DOD with 95-99% purity.

7. A process as claimed in claim 1, wherein the yield of phytosterols obtained is in the range of 80-90% of free sterols available in DOD with 95-99% purity.

8. A process for the preparation of high purity phytosterols from deodourizer distillate from vegetable oils, substantially as herein described with reference to the examples accompanying this specification.