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Process capable of simultaneously producing and separating high-purity EPA (eicosapentaenoic acid) ethyl ester and high-purity DHA (docosahexaenoic acid) ethyl ester

A high-purity, ethyl ester technology, applied in the field of unsaturated fatty acid purification, can solve the problems of complex process, high cost, and long time consumption, and achieve the effect of overcoming high cost

Active Publication Date: 2013-03-13
成都圆大生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of technique of simultaneously producing and separating high-purity EPA ethyl ester and DHA ethyl ester, can purify and separate EPA ethyl ester and DHA ethyl ester effectively, the EPA ethyl ester and DHA ethyl ester content of obtaining are respectively greater than 90%, and the product has no solvent residue, which can overcome the problems of high cost, complicated process, time-consuming and difficult to guarantee safety in the existing technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The raw fish oil is subjected to supercritical carbon dioxide extraction at a temperature of 50°C and a pressure of 8 MPa for 2 hours, the product of the separation tank is collected as free fatty acid, and the raffinate in the extraction tank is obtained to obtain deacidified fish oil.

[0022] Take 1500mL of absolute ethanol and 5g of sodium ethoxide, stir and mix evenly, add it into a reaction kettle with 1000mL of deacidified fish oil, raise the temperature to 50°C, stir for 4 hours, and then concentrate to recover ethanol. Stand still for 60 minutes, separate glycerol at 75°C under normal pressure, then add pure water to wash at 35°C, separate the water layer, and dry the oil layer in vacuum at 65°C, -0.08~-0.09MPa to obtain fatty acid B ester.

[0023] Ethylated fish oil is subjected to continuous countercurrent extraction with supercritical carbon dioxide at a temperature of 40°C and a pressure of 12 MPa to separate glycerides and small molecule fatty acid ethyl ...

Embodiment 2

[0028] The raw fish oil is subjected to supercritical carbon dioxide extraction at a temperature of 50°C and a pressure of 10 MPa for 2 hours, the product of the separation tank is collected as free fatty acid, and the raffinate in the extraction tank is obtained to obtain deacidified fish oil.

[0029] Take 1200mL of absolute ethanol and 4g of sodium ethoxide, stir and mix evenly, add it into a reaction kettle with 1000mL of deacidified fish oil, raise the temperature to 45°C, stir for 4h, and then concentrate at 75°C to recover ethanol. Stand still for 60 minutes, separate the glycerin under normal pressure, then add pure water to wash at 35°C, separate the water layer, and vacuum-dry at 65°C at -0.08~-0.09MPa to obtain fatty acid ethyl ester.

[0030] Ethylated fish oil is subjected to continuous countercurrent extraction with supercritical carbon dioxide at a temperature of 60°C and a pressure of 14 MPa to separate glycerides and small molecule fatty acid ethyl esters from ...

Embodiment 3

[0035] The raw fish oil is subjected to supercritical carbon dioxide extraction at a temperature of 50°C and a pressure of 9 MPa for 2 hours, the product of the separation tank is collected as free fatty acid, and the raffinate in the extraction tank is obtained to obtain deacidified fish oil.

[0036] Take 2000mL of absolute ethanol and 5g of sodium ethoxide, stir and mix evenly, add it into a reaction kettle with 1000mL of deacidified fish oil, raise the temperature to 60°C, stir for 4 hours, and then concentrate to recover ethanol. Stand still for 60 minutes, separate glycerin at 75°C under normal pressure, then add pure water to wash at 35°C, separate the water layer, and vacuum dry at 65°C at -0.08~-0.09MPa to obtain fatty acid ethyl ester.

[0037] Ethylated fish oil is subjected to continuous countercurrent extraction with supercritical carbon dioxide at a temperature of 60°C and a pressure of 8 MPa to separate glycerides and small molecule fatty acid ethyl esters from f...

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Abstract

The invention discloses a process capable of simultaneously producing and separating high-purity EPA (eicosapentaenoic acid) ethyl ester and high-purity DHA (docosahexaenoic acid) ethyl ester. With crude fish oil as raw material, supercritical fluid extraction, base catalysis and esterification, supercritical counter-current extraction, urea clathration and supercritical rectification are carried out, and EPA ethyl ester and DHA ethyl ester with the purity being more than 90% are obtained respectively. By adopting the process disclosed by the invention, the EPA ethyl ester and the DHA ethyl ester can be effectively purified and separated, and the contents of the obtained EPA ethyl ester and DHA ethyl ester are respectively more than 90%; and no residual solvent exists in the product, preoxidation value is less than 2meq / kg, anisidine value is less than 10, acid value is less than 0.5mgKOH / g, polymer is less than 0.2%, no stearin is contained, and the defects of the prior art that cost is high, process is complex, long time is consumed and safety is difficult to guarantee can be overcome.

Description

technical field [0001] The invention relates to a purification technology of unsaturated fatty acid, in particular to a process for simultaneous production and separation of high-purity EPA ethyl ester and DHA ethyl ester. Background technique [0002] Fish oil contains eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) and other unsaturated fatty acids (collectively referred to as Omega-3), which have the functions of preventing and treating cardiovascular and cerebrovascular diseases, preventing Alzheimer's disease and inhibiting tumors. Etc. curative effect. High-purity EPA ethyl ester can also be used as a raw material in the field of medicine and pharmacy. For example, the drug AMR101 developed by Amarin uses EPA ethyl ester with a purity greater than 96%. This drug is used for the treatment of high triglycerides and mixed dyslipidemia. It has entered the third phase of clinical trials. This drug will become the only Prescription-grade omega-3 fatty acids for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/587C07C67/08C07C67/48
CPCY02P20/54
Inventor 郭春林李鹏婧张勇李沅锴苟荣吴向东
Owner 成都圆大生物科技有限公司
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