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Method for preparing high-purity EPA (eicosapentaenoic acid) ester and DHA (docosahexaenoic acid) ester monomers by supercritical chromatography

A supercritical chromatography and high-purity technology, which is applied in the field of supercritical chromatography to prepare high-purity EPA ester and DHA ester monomer, can solve the problems of heavy metal pollution, heavy metal residue, explosion, etc., achieve high separation and avoid the use of solvents , the effect of high purity

Active Publication Date: 2015-04-29
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN101265185B discloses a preparation method for separating eicosapentaenoic acid methyl ester and docosahexaenoic acid methyl ester with a silver nitrate coated silica gel column to obtain 99.02% DHA methyl ester and 99.61% DPA methyl ester respectively , the yield is greater than 90%, but expensive silver nitrate is used, and it is easy to introduce heavy metal pollution
However, this method requires the raw material to be dissolved in methanol in advance and requires a certain proportion of methanol as a modifier
[0010] To sum up, these methods use a large amount of organic solvents or harmful substances, and there are risks of organic solvents and heavy metal residues and the risk of explosion in the production process. A green process with no solvent consumption is developed to mass-produce the purity of more than 95%. The method of EPA ester and DHA ester monomer is very necessary

Method used

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  • Method for preparing high-purity EPA (eicosapentaenoic acid) ester and DHA (docosahexaenoic acid) ester monomers by supercritical chromatography
  • Method for preparing high-purity EPA (eicosapentaenoic acid) ester and DHA (docosahexaenoic acid) ester monomers by supercritical chromatography
  • Method for preparing high-purity EPA (eicosapentaenoic acid) ester and DHA (docosahexaenoic acid) ester monomers by supercritical chromatography

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The polystyrene / divinylbenzene-type reversed-phase resin filler (10 μm, ) is fully swollen in methanol, and then packed into a chromatographic column of 20×250mm by wet packing method. Control the temperature of the supercritical chromatographic system at 40°C, the pressure at 20MPa, supercritical CO 2 The flow rate is 3mL / min. Load 4 mL of mixed polyunsaturated fatty acid ethyl esters into the chromatographic column, wherein the total mass fraction of EPA ethyl ester+DHA ethyl ester in the mixed polyunsaturated fatty acid ethyl ester raw material is 65%. High-purity EPA ethyl ester and DHA ethyl ester fractions were collected in sections according to the elution curve detected online by the ultraviolet detector. After repeating sample loading 20 times, take a small amount of EPA ethyl ester and DHA ethyl ester products in the collection tank, gas chromatography analysis shows that the purity of EPA ethyl ester is 99.6%, and the purity of DHA ethyl ester is 97.9%. A...

Embodiment 2

[0047] The polystyrene / divinylbenzene type reversed-phase resin filler (20μm, ) is fully swollen in methanol, and then packed into a chromatographic column of 10×250mm by wet packing method. Control the temperature of the supercritical chromatographic system at 50°C, the pressure at 10MPa, and the supercritical CO 2 The flow rate is 2mL / min. Load 2 mL of mixed polyunsaturated fatty acid ethyl esters on the chromatographic column, wherein the total mass fraction of EPA ethyl ester + DHA ethyl ester in the mixed polyunsaturated fatty acid ethyl ester raw material is 80%. High-purity EPA ethyl ester and DHA ethyl ester fractions were collected in sections according to the elution curve detected online by the ultraviolet detector. After repeating sample loading 20 times, a small amount of EPA ethyl ester and DHA ethyl ester products were taken in the collection tank, and analyzed by gas chromatography, the purity of EPA ethyl ester was 99.5%, and the purity of DHA ethyl ester w...

Embodiment 3

[0049] Kromasil 100-10-Phenyl type phenyl silica gel packing (10μm, ) was placed in methanol for ultrasonic dispersion, and then packed into a chromatographic column of 10×150 mm by wet packing method. Control the temperature of the supercritical chromatographic system at 40°C, the pressure at 20MPa, supercritical CO 2 The flow rate is 2mL / min. Load 2mL of mixed polyunsaturated fatty acid methyl esters into the chromatographic column, wherein the total mass fraction of EPA methyl ester + DHA methyl ester in the mixed polyunsaturated fatty acid methyl ester raw material is 65%. High-purity EPA methyl ester and DHA methyl ester fractions were collected in sections according to the elution curve detected online by the ultraviolet detector. After repeating sample loading 20 times, a small amount of EPA methyl ester and DHA methyl ester products were taken in the collection tank, and gas chromatography analysis showed that the purity of EPA methyl ester was 99.6%, and the purity...

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Abstract

The invention discloses a method for preparing high-purity EPA (eicosapentaenoic acid) ester and DHA (docosahexaenoic acid) ester monomers by supercritical chromatography, which comprises the following components: constituting a supercritical chromatographic separation system by using supercritical CO2 as a mobile phase and a reverse phase filler as a stationary phase, and controlling the pressure and temperature of the system so that the CO2 in the system is in the supercritical state; injecting a mixed polyunsaturated fatty acid ester raw material solution into a chromatographic column to perform separation; and collecting the EPA ester and DHA ester fraction with the purity of greater than 95% by using a fraction cutter. The whole process greatly reduces the use of the organic solvent, and adopts the reverse phase chromatographic filler containing rich benzene ring. The method has the advantages of high single-time uploading quantity and high purity. The purity of the collected EPA ester and DHA ester monomer product is 95% above. Thus, the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of chemical separation, in particular to a method for preparing high-purity EPA ester and DHA ester monomers by supercritical chromatography. Background technique [0002] EPA and DHA are the two most important polyunsaturated fatty acids in deep-sea fish oil. They have many unique physiological effects on human health, but there are certain differences in their physiological functions. Both EPA and DHA have the effects of improving blood circulation, softening blood vessels, regulating blood lipids, and lowering blood pressure, but DHA has the unique effects of promoting brain development of fetuses and children, protecting eyesight, and regulating immunity. In addition, EPA has a competitive effect on the intake of arachidonic acid, which is necessary for children's development, and will have adverse effects on children's vision and brain development. Therefore, adding EPA in children's nutrition products ...

Claims

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Application Information

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IPC IPC(8): C07C69/602C07C67/56
CPCC07C67/48C07C67/56C07C69/587Y02P20/54
Inventor 任其龙鲍宗必李敏杨亦文邢华斌苏宝根杨启炜张治国
Owner ZHEJIANG UNIV