Method for improving purity of eicosapentaenoic acid ethyl ester in fish oil

A technology for ethyl eicosapentaenoate and ethyl fatty acid is applied in the field of improving the purity of ethyl eicosapentaenoate in fish oil, and can solve the problems of expensive stationary phase, high cost, not production technology and the like, Achieve the effect of being suitable for large-scale production and utilization, overcoming the difficulty of ensuring safety, and achieving good separation and purification effects

Active Publication Date: 2016-11-16
四川欣美加生物医药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since EPA ethyl ester and DHA ethyl ester are polyunsaturated fatty acid ethyl esters, the number of carbon atoms is similar, the boiling point is similar, and the chemical properties are similar. The general purification and separation methods include urea inclusion method, molecular distillation method, metal salt freezing method, Supercritical method, silver nitrate chromatography, etc., these methods cannot completely separate EPA ethyl ester and DHA ethyl ester no matter one or several combinations
Among them, the HPLC method can achieve complete separation, but the HPLC stationary phase is expensive and cannot be reused infinitely, and a large amount of mobile phase solvents are required for separation and the output is limited, resulting in too high a cost for industrial production, so it is not an ideal production technique
Therefore, the purification and separation method of the above-mentioned EPA ethyl ester and DHA ethyl ester generally has the problems that the separation effect is not good, the process is complicated, and the cost is higher.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] First, mix absolute ethanol and sodium ethoxide evenly, add them into a reaction kettle filled with fish oil, and stir for 6 hours at a temperature of 68° C. to carry out a transesterification reaction. Among them, the mass ratio of fish oil, absolute ethanol and sodium ethylate is 1:3:0.01; the acid value of fish oil is 2.9mgKOH / g.

[0043] Secondly, the mixed solution obtained by transesterification was left to stand for stratification, and the upper layer liquid was concentrated and recovered under the conditions of vacuum degree of -0.09MPa and temperature of 65°C to recover absolute ethanol, then added distilled water for washing, and separated the oil layer to obtain Ethyl esterification products of fatty acids.

[0044] After that, first put ethanol into the urine bag tank, then add urea, stir and dissolve to form a urea solution, then add fatty acid ethyl esterification products to the urea solution, stir at 80°C for 2 hours, then cool and crystallize, and recry...

Embodiment 2

[0048] First, absolute ethanol was added into a reaction kettle equipped with fish oil, then sodium ethoxide was added, and then stirred at a temperature of 68° C. for 3 hours to carry out a transesterification reaction. Among them, the mass ratio of fish oil, absolute ethanol and sodium ethylate is 1:2:0.005; the acid value of fish oil is 2.0mgKOH / g.

[0049] Secondly, the mixed solution obtained by transesterification was left to stand for stratification, and the upper layer liquid was concentrated and recovered under the conditions of vacuum degree of -0.08MPa and temperature of 55°C to recover absolute ethanol, then added distilled water for washing, and separated the oil layer to obtain Ethyl esterification products of fatty acids.

[0050] After that, first put ethanol into the urine bag tank, then add urea, stir and dissolve to form a urea solution, then add fatty acid ethyl esterification products to the urea solution, stir at 70°C for 1 hour, then cool and crystallize...

Embodiment 3

[0054] First, absolute ethanol was added into a reaction kettle equipped with fish oil, then sodium ethoxide was added, and then stirred at a temperature of 68° C. for 4 hours to carry out a transesterification reaction. Among them, the mass ratio of fish oil, absolute ethanol and sodium ethylate is 1:2.5:0.008; the acid value of fish oil is 1.5mgKOH / g.

[0055] Secondly, the mixed solution obtained by transesterification was left to stand for stratification, and the upper layer liquid was concentrated and recovered under the conditions of vacuum degree of -0.08MPa and temperature of 60°C to recover absolute ethanol, then added distilled water for washing, and separated the oil layer to obtain Ethyl esterification products of fatty acids.

[0056] After that, first put ethanol into the urine bag tank, then add urea, stir and dissolve to form a urea solution, then add fatty acid ethyl esterification products to the urea solution, stir at 75°C for 1.5h, then cool and crystallize...

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Abstract

The invention discloses a method for improving purity of eicosapentaenoic acid ethyl ester in fish oil. The method comprises steps as follows: the fish oil is subjected to transesterification, and a fatty acid ethyl esterification product is obtained; the fatty acid ethyl esterification product is subjected to urea inclusion, and a urea inclusion mixture is obtained; the urea inclusion mixture is subjected to at least three stages of molecular distillation, and a molecular distillation product is obtained; the molecular distillation product is subjected to rectification. According to the method, the technology is simple, the content of eicosapentaenoic acid ethyl ester in the fish oil can be effectively increased, meanwhile, the content of docosahexaenoic acid ethyl ester is reduced, and the separation effect is good, so that eicosapentaenoic acid ethyl ester can be better applied to industrial production.

Description

technical field [0001] The invention relates to the technical field of fish oil component purification, in particular to a method for improving the purity of ethyl eicosapentaenoate in fish oil. Background technique [0002] Crude fish oil is rich in w-3 polyunsaturated fatty acids, among which eicosapentaenoic acid (EPA) and docosahexaenoic acid (DHA) are the main content, but EPA and DHA have different application fields: EPA is mainly used to lower blood fat, lower blood pressure, and prevent atherosclerosis; DHA is mainly used to enhance memory and prevent myopia. EPA and DHA exist in the form of EPA ethyl ester and DHA ethyl ester in fish oil products, so as to purify and separate fish oil The EPA ethyl ester and DHA ethyl ester in DHA are the focus of current research. However, since EPA ethyl ester and DHA ethyl ester are polyunsaturated fatty acid ethyl esters, the number of carbon atoms is similar, the boiling point is similar, and the chemical properties are simil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C67/62C07C67/54C07C69/587
CPCC07C67/08C07C67/54C07C67/62C07C69/587
Inventor 杨国文
Owner 四川欣美加生物医药有限公司
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