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Process for preparing and separating methyl docosapentaenoate and methyl docosahexenoate

A kind of technology of methyl docosahexaenoate and methyl docosahexaenoate, applied in the field of preparation and separation of methyl docosahexaenoate and methyl docosahexaenoate , which can solve the problems of complicated brine shrimp meal process and lower yield, and achieve the effect of short heating time, avoided loss and high yield.

Active Publication Date: 2008-09-17
NANGTONG HAODI ANTICORROSION EQUIP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Application No. 03113397.5 discloses a method for preparing DHA value through marinated shrimp protein powder. The process of preparing marinated shrimp powder in the early stage of this method is complicated, and ethyl esterification method is also used, which reduces the yield

Method used

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  • Process for preparing and separating methyl docosapentaenoate and methyl docosahexenoate
  • Process for preparing and separating methyl docosapentaenoate and methyl docosahexenoate
  • Process for preparing and separating methyl docosapentaenoate and methyl docosahexenoate

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Embodiment 1

[0026] Apply silver nitrate column method to prepare high-purity docosapentaenoic acid (DPA) methyl ester and docosahexaenoic acid (DHA) methyl ester, comprising the steps:

[0027] 1) Preparation of crude fatty acid: Take 500g of microalgae oil, 50g of KOH, and 1000ml of methanol, put them into a three-necked flask, use nitrogen as a protective gas, stir continuously, and reflux in a water bath at 60-120°C for 1-4 hours. After most of the solvent was removed by rotary evaporation, 6mol / L hydrochloric acid was added to acidify. After the fatty acid was extracted three times with 300ml petroleum ether, the ether phase was washed with 5% NaCl aqueous solution until the washing liquid was neutral. Add anhydrous Na 2 SO 4 Absorb the residual water in the ether phase, and remove the solvent by rotary evaporation at 60°C to obtain the crude fatty acid.

[0028] 2) Preparation of DPA and DHA mixed fatty acid: Take 100g crude fatty acid, 30g~300g urea, 600ml methanol and mix, reflux...

Embodiment 2

[0032] Basic technology is with embodiment 1, and concrete operation parameter is as follows:

[0033] 1) Preparation of crude fatty acid: Take 250 g of seaweed oil, 50 g of KOH, and 500 ml of methanol, put them into a three-necked flask, use nitrogen as a protective gas, keep stirring, and reflux in a water bath at 60-120° C. for 2 hours. After most of the solvent was removed by rotary evaporation, 6mol / L hydrochloric acid was added to acidify. After the fatty acid was extracted three times with 300ml petroleum ether, the ether phase was washed with 5% NaCl aqueous solution until the washing liquid was neutral. Add anhydrous Na 2 SO 4 Absorb the residual water in the ether phase, and remove the solvent by rotary evaporation at 60°C to obtain the crude fatty acid.

[0034] 2) Preparation of DPA and DHA mixed fatty acid: Take 75g of crude fatty acid, 150g of urea, and 600ml of methanol, mix them, reflux in a water bath at 50-80°C for 15 minutes, cool and crystallize at -10°C ...

Embodiment 3

[0038] Basic technology is with embodiment 1, and concrete operation parameter is as follows:

[0039] 1) The preparation of crude fatty acid, the methyl esterification of the preparation of DPA and DHA mixed fatty acid and DPA and DHA mixture are the same as embodiment 2.

[0040] 2) silver nitrate column method obtains DPA methyl ester and DHA methyl ester respectively: prepare Ag by the method in example 1 + Silica gel, weigh 100g of the prepared Ag + Silica gel, wet packed column with n-hexane as eluent. Take DPA methyl ester and DHA methyl ester mixture 0.5g sample. Respectively with 0.5% acetone n-hexane solution 2000ml, 10% acetone n-hexane solution 500ml, 15% acetone n-hexane solution 1000ml elution, each 60ml as a sample, evaporated to remove solvent, detected by gas chromatography, combined the same group points, high-purity DPA methyl ester and DHA methyl ester can be obtained respectively.

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Abstract

The invention relates to a preparation and separation method of docosapentaenoic acid methyl ester and docosahexaenoic acid methyl ester. Microalgae oil is used as raw material to prepare docosapentaenoic acid and docosahexaenoic acid which are mixed with fatty acid to prepare the docosapentaenoic acid methyl ester and the docosahexaenoic acid methyl ester. The separation method of the the docosapentaenoic acid methyl ester and the docosahexaenoic acid methyl ester provided by the method adopts a silver nitrate column method of separating. In the silver nitrate column method, the quality of the methyl ester sample introduction of the mixed fatty acid is 0.5 percent to 10 percent of the quality of filled silver nitrate blangel; elution gradient is n-hexane solution containing acetone the content of which is 0.5 percent to 15 percent; the elution speed is 0.5 to 5ml / min. The preparation and separation method utilizes the silver nitrate column method to obtain the high purity docosapentaenoic acid methyl ester and the high purity docosahexaenoic acid methyl ester, wherein, the content of DPA is raised from 20.32 percent in raw oil to 99.61 percent, the content of DHA is raised from 44.83 percent to 99.02 percent, and the yield rate by using the silver nitrate column method can reach more than 90 percent.

Description

technical field [0001] The invention relates to a preparation and separation method of docosapentaenoic acid (DPA) methyl ester and docosahexaenoic acid (DHA) methyl ester. Background technique [0002] Microalgae are a class of marine microorganisms that contain chlorophyll, and their growth habits are the same as those of algae. Studies have shown that microalgal fat is rich in omega-3 polyene fatty acids. Years of research in the medical field have confirmed that omega-3 polyene fatty acids have a variety of unique physiological effects on human health, especially EPA (eicosapentaenoic acid), DPA (docosapentaenoic acid) and DHA ( Docosahexaenoic acid), its unique health benefits are recognized and accepted by more and more people. Most of the active ingredients in the omega-3 polyene fatty acid health products currently used by humans come from deep sea fish oil and seal oil. With the shortage of marine fishery resources in the world and the existence of problems such ...

Claims

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Application Information

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IPC IPC(8): C07C69/587C07C67/08
Inventor 丁辉王嵩张艳华徐世民
Owner NANGTONG HAODI ANTICORROSION EQUIP
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