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High-purity DHA algae oil ethyl ester and preparation method for transferring high-purity DHA algae oil ethyl ester into glyceride

An oil ethyl ester and ethyl esterification technology, applied in the field of DHA glycerides, can solve the problems of low smoke point of ester products, complicated product process, low DHA percentage content, etc., to improve reaction efficiency and reaction speed, improve DHA content, the effect of increasing the percentage content

Active Publication Date: 2014-06-25
JIANGSU ZHONGBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, in the recognized technology, the processed and purified fish oil or algae oil products are mainly esterified products, such as ethyl ester or methyl ester, by esterification process. As we all know, ester products are not natural structures, and their bioabsorption The efficiency and utilization are not high, and it is easy to generate ethanol or methanol in the body, which has certain side effects; and the smoke point of ester products is low and easy to oxidize
The above reasons cause the medicinal and health effects of ester type DHA to be poor, which limits the application field of DHA
At the same time, some products need to be further processed and refined, resulting in complicated processes for subsequent products
[0003] Domestic Tianjin University reports two patents CN101260344A and CN101265185A, the former adopts urea embedding method to increase Schizochytrium DHA from 44.83% to 64.46%, but the percentage content of DHA is still low, and the latter uses silver nitrate method to increase DHA from 44.83% to 64.46%. % increased to 99.02%, but AgNO 3 More expensive and not easy to industrialize

Method used

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  • High-purity DHA algae oil ethyl ester and preparation method for transferring high-purity DHA algae oil ethyl ester into glyceride

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Experimental program
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Effect test

Embodiment 1

[0029] (1) Ethyl esterification of DHA oil: Dissolve 40g KOH in 1.30kg ethanol, mix 4kg Cryptoninella DHA oil (DHA accounts for 43.48%) and KOH-ethanol solution fully, under the condition of nitrogen filling, Heating and refluxing in a 60°C water bath for 1 hour; cooling to room temperature under nitrogen-filled conditions, standing for stratification, and then taking the upper ethylesterified layer to recover ethanol under reduced pressure distillation at 60°C and -0.1Mpa to obtain the ethylesterified product. Wash with warm water at 40°C until the washing water is neutral, and then rinse with anhydrous Na 2 SO 4 Dry to obtain crude DHA ethyl ester;

[0030] (2) Purification of DHA ethyl ester by secondary molecular distillation method: The crude DHA ethyl ester product enters the molecular distillation device at a feed rate of 5.0g / min through the feed pump for degassing treatment, and the degassing temperature is 70°C, and the heavy components are collected and repeated fo...

Embodiment 2

[0032] (1) Ethyl esterification of DHA oil: Dissolve 32g KOH in 1.45kg ethanol, mix 4kg Crypthecodinium algae DHA oil (43.48% DHA) with KOH-ethanol solution, under the condition of nitrogen Heating and refluxing in a 50°C water bath for 2 hours; cooling to room temperature under nitrogen-filled conditions, standing for stratification, and then taking the upper ethyl esterified layer to recover ethanol under reduced pressure distillation at 60°C and -0.1 Mpa, and the obtained ethyl esterification product was Wash with warm water at 40°C until the washing water is neutral, and then rinsed with anhydrous Na 2 SO 4 Dry to obtain crude DHA ethyl ester;

[0033] (2) Purification of DHA ethyl ester by secondary molecular distillation method: The crude DHA ethyl ester product enters the molecular distillation device at a feed rate of 8.0g / min through the feed pump for degassing treatment, the degassing temperature is 80°C, and the heavy components are collected for repeated distillat...

Embodiment 3

[0035] (1) Ethyl esterification of DHA oil: Dissolve 48g KOH in 1.25kg ethanol, mix 4kg Cryptoninella DHA oil (43.48% DHA) with KOH-ethanol solution, under nitrogen Heating and refluxing in a 70°C water bath for 1 hour; cooling to room temperature under nitrogen-filled conditions, standing for stratification, and then taking the upper ethylesterified layer to recover ethanol under reduced pressure distillation at 60°C and -0.1Mpa. Wash with warm water at 40°C until the washing water is neutral, and then washed with anhydrous Na 2 SO 4 Dry to obtain crude DHA ethyl ester;

[0036] (2) Purification of DHA ethyl ester by secondary molecular distillation method: The crude DHA ethyl ester product enters the molecular distillation device at a feed rate of 20g / min through the feed pump for degassing treatment, the degassing temperature is 80°C, and the heavy components are collected and repeated for distillation 1 The heavy components obtained by degassing were subjected to first-l...

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Abstract

The invention discloses a DHA algae oil ethyl ester and a preparation method thereof. The method comprises the following steps: carrying out ethyl-esterifying on crypthecodinium cohnii DHA grease and then purifying trough a secondary molecular distillation method to obtain high-purity DHA ethyl ester. The invention further discloses a DHA glyceride and a method for transferring the DHA algae oil ethyl ester into glyceride. The method comprises the following steps: mixing the DHA algae oil ethyl ester with glycerinum in a material tank, feeding the mixed material in a reactor having immobilized lipase, performing transesterification to replace out the ethanol, recycling through a condenser, and flowing the reacted mixture back to the material tank, circularly reacting for 5-60 hours, and finally returning to the material tank, wherein the glyceride product is obtained by performing molecule distillation on the material. The method disclosed by the invention is suitable for the industrial production, the DHA greased produced from the microorganism is used as the raw material, the percent content of the DHA is greatly improved, the ethyl ester is transferred into the glyceride, the ethanol is avoided, the side effect after eating is not generated, and the utilization degree of the DHA algae oil ethyl ester in vivo is effectively improved.

Description

technical field [0001] The invention relates to DHA algae oil ethyl ester and DHA glyceride prepared by using DHA algae oil ethyl ester as a raw material, in particular to a DHA algae oil ethyl ester prepared by using Cryptodinia algae DHA oil as a raw material and preparation thereof Method, and DHA glyceride prepared by using DHA algal oil ethyl ester as raw material and preparation method thereof. Background technique [0002] Docosahexaenoic acid (DHA) has important physiological activities and can lower blood lipids, lower blood pressure, and improve intelligence. It has broad development and application prospects as an important raw material for medicines and health food. The DHA content of fish oil or algae oil is low. The DHA content of algae oil accounts for 30%-50% of the total fatty acid, and there is less in fish oil. With the continuous progress of science and technology and the development of the medical and health care products industry, people have higher an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/587C07C67/54C07C67/08C12P7/64
CPCC07C67/03C07C67/54C07C69/587C12P7/6454C12P7/6472
Inventor 邢华忠吴建平邢光才周颖李维思
Owner JIANGSU ZHONGBANG PHARMA
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