High-purity dha algae oil ethyl ester and its conversion into glyceride preparation method

A technology of oil ethyl ester and ethyl esterification, 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: 2016-05-04
JIANGSU ZHONGBANG PHARMA
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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 the urea embedding method to increase the Schizochytrium DHA from 44.83% to 64.46%, but the DHA percentage content is still low, and the latter adopts the silver nitrate method to increase the 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 its conversion into glyceride preparation method

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Experimental program
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Effect test

Embodiment 1

[0029] (1), ethyl esterification of DHA oil: get 40gKOH and be dissolved in 1.30kg ethanol, after fully mixing with KOH-ethanol solution with 4kg cryptodinoflagellate DHA oil (DHA accounts for 43.48%), under the condition of filling nitrogen, in Heating and refluxing in a water bath at 60°C for 1 hour; cooling to room temperature under the condition of nitrogen filling, standing for stratification, taking the upper ethyl esterification layer and distilling under reduced pressure at 60°C and -0.1MPa to recover ethanol, and the ethyl esterification product obtained is Wash with warm water at 40°C until the washing water is neutral, and wash with anhydrous Na 2 SO 4 Dried to obtain the crude product of DHA ethyl ester;

[0030] (2) Purification of DHA ethyl ester by two-stage molecular distillation method: the crude product of DHA ethyl ester enters the molecular distillation device at a feed rate of 5.0g / min through a feed pump for degassing treatment. The degassing temperature...

Embodiment 2

[0032] (1) Ethyl esterification of DHA oil: get 32gKOH and dissolve in 1.45kg ethanol, after fully mixing 4kg cryptodininosaur DHA oil (DHA accounts for 43.48%) and KOH-ethanol solution, under the condition of filling nitrogen, at 50 Heating and refluxing in a water bath at ℃ for 2 hours; cooling to room temperature under the condition of nitrogen filling, standing for stratification, taking the upper ethyl esterification layer and distilling under reduced pressure at 60 °C and -0.1MPa to recover ethanol. ℃ warm water wash until the washing water is neutral, through anhydrous Na 2 SO 4 Dried to obtain the crude product of DHA ethyl ester;

[0033] (2) Purification of DHA ethyl ester by secondary molecular distillation method: the crude product of DHA ethyl ester enters the molecular distillation device through the feed pump at a feed rate of 8.0g / min for degassing treatment. The degassing temperature is 80°C, and the heavy components are collected and distilled 1 time; the h...

Embodiment 3

[0035] (1) Ethyl esterification of DHA oil: get 48gKOH and dissolve in 1.25kg ethanol, after fully mixing 4kg cryptodininosaur DHA oil (DHA accounts for 43.48%) and KOH-ethanol solution, under the condition of filling nitrogen, at 70 Heating and refluxing in a water bath at ℃ for 1 hour; cooling to room temperature under the condition of nitrogen filling, standing for stratification, taking the upper ethyl esterification layer, and distilling under reduced pressure at 60 °C and -0.1MPa to recover ethanol. ℃ warm water wash until the washing water is neutral, through anhydrous Na 2 SO 4 Dried to obtain the crude product of DHA ethyl ester;

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

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Abstract

The invention discloses a DHA algae oil ethyl ester and a preparation method thereof. Firstly, the DHA oil ethyl ester of Cryptodinium algae is esterified and then purified by a secondary molecular distillation method to obtain high-purity DHA ethyl ester. The invention also discloses a method for converting DHA glyceride and DHA algae oil ethyl ester into DHA glyceride. DHA algae oil ethyl ester and glycerin are mixed in a material tank, and the mixed material enters a reaction chamber equipped with immobilized lipase. The ethanol displaced by the transesterification reaction is recovered by the condenser, and then the reaction mixture is returned to the material tank, and after 5 to 60 hours of circular reaction, it is finally returned to the material tank; the obtained material is molecularly distilled to obtain a glyceride-type product. The present invention is suitable for industrialized production, adopts DHA oil produced by microorganisms as raw material, greatly increases the percentage content of DHA, converts the ethyl ester type into the glyceride type, does not contain ethanol, has no side effects after eating, and effectively improves its in vivo utilization.

Description

technical field [0001] The present invention relates to DHA algal oil ethyl ester and DHA glyceride prepared by using DHA algal oil ethyl ester as raw material, in particular to DHA algal oil ethyl ester prepared by using Cryptidinosa DHA oil as raw material and its preparation method, and DHA glyceride prepared from DHA algae oil ethyl ester as a raw material and a preparation method thereof. Background technique [0002] Docosahexaenoic acid (DHA) has important physiological activities, can lower blood fat, lower blood pressure, improve intelligence and other effects, and it has broad development and application prospects as an important raw material of medicine and health food. The DHA content of fish oil or algae oil is relatively low, and DHA in algae oil accounts for 30%-50% of the total fatty acid content, and less in fish oil. With the continuous advancement of science and technology and the development of the pharmaceutical and health care products industry, people...

Claims

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Application Information

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Patent Type & Authority Patents(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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