A method for preparing chromatographically purified alpha-linolenic acid ethyl ester

A technology for ethyl linolenate and chromatographic purification, which is applied in the field of preparation of chromatographic purification of α-ethyl linolenate, can solve the problems of high energy consumption, complex process, low purification efficiency of α-ethyl linolenate, etc., and achieve low energy consumption , simple process and stable stationary phase

Active Publication Date: 2015-12-02
HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention aims to solve the problems of low purification efficiency of ethyl α-linolenic acid, complicated process and high energy consumption, and studies a method for purifying ethyl α-linolenic acid by using preparative chromatographic technology

Method used

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  • A method for preparing chromatographically purified alpha-linolenic acid ethyl ester
  • A method for preparing chromatographically purified alpha-linolenic acid ethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 1. Column packing: put the stationary phase ODS with a particle size of 30-50 μm in ethanol, stir and remove air bubbles, and then evenly load the stationary phase ODS into the prepared chromatographic column. The diameter of the chromatographic column is 15mm and the length is 460mm. Rinse with eluent for 24 hours, open the preparative chromatographic column for secondary filling, rinse again for 24 hours, open the preparative chromatographic column for third filling, and obtain the packed preparative chromatographic column after the stationary phase ODS is compacted;

[0020] 2. Feed: Feed through the six-port sampling valve, the feed concentration is 100% α-ethyl linolenate, and the feed volume is 4mL;

[0021] 3. Elution: pump the eluent with constant pressure and constant flow, the eluent is methanol aqueous solution with a volume fraction of 98%, the amount of eluent is 300mL, and the elution flow rate is 2mL / min; the pressure of the preparation column is 0.4MPa; ...

Embodiment 2

[0025] 1. Column packing: operate according to step 1 in Example 1;

[0026] 2. Feed: Feed through the six-port sampling valve, the feed concentration is 100% α-ethyl linolenate, and the feed volume is 4mL;

[0027] 3. Elution: pump the eluent with constant pressure and constant flow, the eluent is 100% methanol, the amount of eluent is 240mL, and the elution flow rate is 4mL / min; the pressure of the preparation column is 0.3MPa; the column temperature is 30°C;

[0028] 4. Collection: The eluted fraction is collected in sections, and the collection is divided into two times. The first collection is mainly α-linolenic acid ethyl ester component, and 128mL is collected; the second collection is mainly other components, and 112mL is collected. ;

[0029] 5. Recovery of eluent: The eluent was recovered by concentration under reduced pressure, and the purity of ethyl α-linolenic acid was 91.3%, and the yield was 73.2%.

Embodiment 3

[0031] 1. Column packing: operate according to step 1 in Example 1;

[0032] 2. Feed: Feed through the six-port sampling valve, the feed concentration is 100% α-ethyl linolenate, and the feed volume is 4mL;

[0033] 3. Elution: pump the eluent with constant pressure and constant flow, the eluent is 100% methanol, the amount of eluent is 260mL, and the elution flow rate is 4mL / min; the pressure of the preparation column is 0.3MPa; the column temperature is 30°C;

[0034] 4. Collection: The eluted fraction is collected in sections, and the collection is divided into two times. The first collection is mainly α-linolenic acid ethyl ester component, and 152 mL is collected; the second collection is mainly other components, and 108 mL is collected. ;

[0035] 5. Recovery of eluent: Concentrate under reduced pressure to recover the eluent, and the purity of ethyl α-linolenic acid is 85.5%, and the yield is 84.8%.

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Abstract

The invention discloses a method for preparing chromatographically purified ethyl alpha-linolenate. The method comprises the following steps of: purifying an ethyl alpha-linolenate crude product with content of not less than 50% as a raw material by preparative chromatography separation equipment, wherein methyl alcohol or ethyl alcohol is used as an eluent, the working temperature of a system is set to 25-30 DEG C, ODS is used as a chromatographic stationary phase, materials are charged by a six-way sampling valve, and the eluent is charged by a constant-pressure and constant-flow pump; fractionally collecting the eluted fractions, and recovering the eluent by reduced pressure concentration to obtain high-purity ethyl alpha-linolenate, wherein the yield is high. The whole process is simple in flow, low in production cost, low in production energy consumption, zero-emission and pollution-free, capable of continuously producing and increasing production efficiency, and suitable for large-scale production. The ethyl alpha-linolenate purified by the method is high in purity, low in solvent residue, and capable of meeting the needs of industries such as chemical analysis, medicines and health products.

Description

technical field [0001] The invention relates to a purification technology of alpha-linolenic acid ethyl ester, in particular to a technology for preparing chromatographically purified alpha-linolenic acid ethyl ester. Background technique [0002] α-linolenic acid is octadecadenoic acid. As an omega-3 unsaturated fatty acid, it has significant pharmacological effects and nutritional value. Symptoms and so on have a certain effect. The derivative of α-linolenic acid, α-linolenic acid ethyl ester, has the effects of treating obesity, inhibiting allergies, and preventing cardiovascular and cerebrovascular diseases. Long-term consumption can prolong life. It can be used in food additives, high-efficiency dispersants, cosmetics, advanced dry It has been effectively applied in oil and oil recovery processes. Therefore, the high-purity products of α-linolenic acid ethyl ester are being researched at home and abroad for use in pharmaceuticals, life sciences and chemistry. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/587C07C67/48C07C67/56
CPCC07C67/48C07C67/56C07C69/587
Inventor 李良玉于伟李朝阳贾鹏禹张丽萍曹龙奎王学群吕获柱
Owner HEILONGJIANG BAYI AGRICULTURAL UNIVERSITY
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