CN103242965A - Method for extracting and purifying alpha-linolenic acid - Google Patents
Method for extracting and purifying alpha-linolenic acid Download PDFInfo
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- CN103242965A CN103242965A CN2013102123872A CN201310212387A CN103242965A CN 103242965 A CN103242965 A CN 103242965A CN 2013102123872 A CN2013102123872 A CN 2013102123872A CN 201310212387 A CN201310212387 A CN 201310212387A CN 103242965 A CN103242965 A CN 103242965A
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Abstract
The invention relates to a method for extracting and purifying alpha-linolenic acid. The method comprises the following steps of: 1, pre-treating a raw material of alpha-linolenic acid raw oil; 2, carrying out ethyl esterification on the pre-treated alpha-linolenic acid raw oil; 3, preliminarily purifying the alpha-linolenic acid by using a gradient freezing method to obtain the alpha-linolenic acid of which the purity is greater than 70%; and 4, further purifying the alpha-linolenic acid by using a three-stage molecular distillation method to obtain the alpha-linolenic acid of which the purity is 90.5-92.5%. The method has the beneficial effects that the purity of the product is high, the alpha-linolenic acid of which the purity is 90.5-92.5% is obtained, and a pure physical extracting and purifying method is adopted to replace the conventional urea inclusion process and ensure that the alpha-linolenic acid product does not have urea residues and toxic substances.
Description
Technical field
The present invention relates to a kind of extracting and purifying method of unsaturated fatty acids, relate in particular to a kind of method of extracting purifying alpha-linolenic acid.
Background technology
Alpha-linolenic acid is the necessary polyunsaturated fatty acid of a kind of human body, is the life core substance.The scientific research result of authority research institution shows, its meta-bolites EPA and DHA etc. have prophylactic effect to kind of a disease surplus 50, and can suppress the generation of diene prostaglandin(PG), and the diene prostaglandin(PG) can suppress immune cell function; Alpha-linolenic acid is as must regulating lipid metabolism by lipid acid, and disorders of lipid metabolism can cause hypoimmunity.
The method of present existing extraction purifying alpha-linolenic acid is urea adduct method mostly, and it is residual that this kind method has urea, and HUMAN HEALTH is produced harm, and country progressively limits the extraction purifying that urea adduct method is used for alpha-linolenic acid at present.
Summary of the invention
The present invention is directed to above-mentioned the deficiencies in the prior art, a kind of method of extracting purifying alpha-linolenic acid is provided.This method need not passed through the urea clathration step, has avoided urea residual, does not have toxic side effect.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of method of extracting purifying alpha-linolenic acid, carry out according to following steps:
The first step: alpha-linolenic acid stock oil is carried out pre-treatment: described pre-treatment step comprises commercially available alpha-linolenic acid stock oil admission check, impurity elimination and coarse filtration;
Second step: pretreated alpha-linolenic acid stock oil carry out ethyl esterization: the ethanol of pretreated alpha-linolenic acid stock oil and 95% is mixed, and under basic catalyst, vacuum state condition, 70-75 ℃ was reacted 1-2 hour, separated through washing again;
The 3rd step: utilize gradient freezing method preliminary purification alpha-linolenic acid: the product that the fs obtained for second step is down to 0 ℃, is incubated 1h, is washed suction filtration from original temperature, subordinate phase from 0 ℃ be down to-10 ℃, the insulation 1h, the washing suction filtration, phase III from-10 ℃ be down to-15 ℃, the insulation 1h, the washing suction filtration, the quadravalence section from-15 ℃ be down to-20 ℃, the insulation 1h, the washing suction filtration, five-stage is down to-30 ℃, insulation 1h, washing suction filtration from-20 ℃, obtains purity greater than 70% alpha-linolenic acid;
The 4th step: utilize three grades of molecule distillation method alpha-linolenic acid of further purifying: three grades of molecule distil process parameters are, send purity to molecular still greater than 70% alpha-linolenic acid and carry out three grades of molecule distillations, 90-100 ℃ of first step molecular distillation temperature, pressure 1.0-1.5Pa, second stage distillation temperature 115-120 ℃, pressure 1.0-1.5Pa, 120-125 ℃ of third stage distillation temperature, pressure 1.0-1.5Pa obtain the alpha-linolenic acid that purity is 90.5-92.5%.
Described alpha-linolenic acid stock oil is a kind of in linseed oil, Purple Perilla Seed Oil, Eucommia Oil, Oleum Hippophae, Fructus Zanthoxyli oil, the Hemp Seed oil.
Compared with prior art, beneficial effect of the present invention: alpha-linolenic acid product purity height, solidify a little difference according to each lipid acid in the alpha-linolenic acid stock oil, adopt the gradient freezing method, differing temps repeated freezing, suction filtration obtain purity greater than 70% alpha-linolenic acid; According to the difference of each lipid acid boiling point in the alpha-linolenic acid stock oil, carry out three grades of molecule distillations respectively at differing temps, obtaining purity is 90.5-92.5%.The pure physics extracting and purifying method of the present invention has been removed traditional urea clathrate process, and it is residual to make the product alpha-linolenic acid not have urea, no toxic substance.
Embodiment
Below principle of the present invention and feature are described, institute only gives an actual example and to be used for explaining the present invention, is not for restriction scope of the present invention.
Embodiment 1
A kind of method of extracting purifying alpha-linolenic acid, carry out according to following steps:
The first step: alpha-linolenic acid stock oil is carried out pre-treatment: described pre-treatment step comprises commercially available alpha-linolenic acid stock oil admission check, impurity elimination and coarse filtration;
Second step: pretreated alpha-linolenic acid stock oil carry out ethyl esterization: the ethanol of pretreated alpha-linolenic acid stock oil and 95% is mixed, and under basic catalyst, vacuum state condition, 70-75 ℃ was reacted 1-2 hour, separated through washing again;
The 3rd step: utilize gradient freezing method preliminary purification alpha-linolenic acid: the product that the fs obtained for second step is down to 0 ℃, is incubated 1h, is washed suction filtration from original temperature, subordinate phase from 0 ℃ be down to-10 ℃, the insulation 1h, the washing suction filtration, phase III from-10 ℃ be down to-15 ℃, the insulation 1h, the washing suction filtration, the quadravalence section from-15 ℃ be down to-20 ℃, the insulation 1h, the washing suction filtration, five-stage is down to-30 ℃, insulation 1h, washing suction filtration from-20 ℃, obtains purity greater than 70% alpha-linolenic acid;
The 4th step: utilize three grades of molecule distillation method alpha-linolenic acid of further purifying: three grades of molecule distil process parameters are, send purity to molecular still greater than 70% alpha-linolenic acid and carry out three grades of molecule distillations, 90-100 ℃ of first step molecular distillation temperature, pressure 1.0-1.5Pa, second stage distillation temperature 115-120 ℃, pressure 1.0-1.5Pa, 120-125 ℃ of third stage distillation temperature, pressure 1.0-1.5Pa obtain the alpha-linolenic acid that purity is 90.5-92.5%.
Wherein alpha-linolenic acid stock oil is a kind of in linseed oil, Purple Perilla Seed Oil, Eucommia Oil, Oleum Hippophae, Fructus Zanthoxyli oil, the Hemp Seed oil.
The present invention extracts alpha-linolenic acid from alpha-linolenic acid stock oil, also can be applicable to purification enrichment DHA and EPA from fish oil.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from which point, above-mentioned embodiment of the present invention all can only be thought can not limit the present invention to explanation of the present invention, claims have been pointed out scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, in the implication suitable with claims of the present invention and any change in the scope, all should think to be included in the scope of claims.
Claims (2)
1. a method of extracting purifying alpha-linolenic acid is characterized in that, carries out according to following steps:
The first step: alpha-linolenic acid stock oil is carried out pre-treatment: described pre-treatment step comprises commercially available alpha-linolenic acid stock oil admission check, impurity elimination and coarse filtration;
Second step: pretreated alpha-linolenic acid stock oil carry out ethyl esterization: the ethanol of pretreated alpha-linolenic acid stock oil and 95% is mixed, and under basic catalyst, vacuum state condition, 70-75 ℃ was reacted 1-2 hour, separated through washing again;
The 3rd step: utilize gradient freezing method preliminary purification alpha-linolenic acid: the product that the fs obtained for second step is down to 0 ℃, is incubated 1h, is washed suction filtration from original temperature, subordinate phase from 0 ℃ be down to-10 ℃, the insulation 1h, the washing suction filtration, phase III from-10 ℃ be down to-15 ℃, the insulation 1h, the washing suction filtration, the quadravalence section from-15 ℃ be down to-20 ℃, the insulation 1h, the washing suction filtration, five-stage is down to-30 ℃, insulation 1h, washing suction filtration from-20 ℃, obtains purity greater than 70% alpha-linolenic acid;
The 4th step: utilize three grades of molecule distillation method alpha-linolenic acid of further purifying: three grades of molecule distil process parameters are, send purity to molecular still greater than 70% alpha-linolenic acid and carry out three grades of molecule distillations, 90-100 ℃ of first step molecular distillation temperature, pressure 1.0-1.5Pa, second stage distillation temperature 115-120 ℃, pressure 1.0-1.5Pa, 120-125 ℃ of third stage distillation temperature, pressure 1.0-1.5Pa obtain the alpha-linolenic acid that purity is 90.5-92.5%.
2. a method of extracting purifying alpha-linolenic acid is characterized in that, described alpha-linolenic acid stock oil is a kind of in linseed oil, Purple Perilla Seed Oil, Eucommia Oil, Oleum Hippophae, Fructus Zanthoxyli oil and the Hemp Seed oil.
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Cited By (9)
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| CN103864614A (en) * | 2014-03-20 | 2014-06-18 | 江苏中邦制药有限公司 | Method for separating and purifying DHA (docosahexaenoic acid) ethyl ester from DHA oil produced by microbial fermentation |
| CN104719891A (en) * | 2015-03-05 | 2015-06-24 | 陈学沛 | Health product capable of improving immunity |
| CN104744235A (en) * | 2015-02-28 | 2015-07-01 | 陈学沛 | Process for preparing alpha-linolenic acid |
| CN105341929A (en) * | 2015-12-02 | 2016-02-24 | 烟台燕园科玛健康产业有限公司 | Health-care food composition capable of alleviating asthenopia |
| CN105695093A (en) * | 2016-02-14 | 2016-06-22 | 青海福来喜得生物科技股份有限公司 | Method for extracting high-purity flaxseed oil by aid of molecular distillation processes |
| CN105831766A (en) * | 2016-03-25 | 2016-08-10 | 江苏自然之道生物科技有限公司 | Blood-fat-reducing product and preparation method thereof |
| CN108753455A (en) * | 2018-07-20 | 2018-11-06 | 广州利众生物科技有限公司 | A method of extracting high-purity linseed oil using molecularly distilled |
| CN110157541A (en) * | 2019-05-23 | 2019-08-23 | 河南农业大学 | A kind of woody alpha-linolenic acid concentrated method |
| CN114381333A (en) * | 2020-10-20 | 2022-04-22 | 云南汉盟制药有限公司 | Preparation method of hemp seed oil with high polyunsaturated fatty acid content |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864614A (en) * | 2014-03-20 | 2014-06-18 | 江苏中邦制药有限公司 | Method for separating and purifying DHA (docosahexaenoic acid) ethyl ester from DHA oil produced by microbial fermentation |
| CN103864614B (en) * | 2014-03-20 | 2015-11-25 | 江苏中邦制药有限公司 | The method of separation and purification DHA-EE from the DHA grease of fermentable |
| CN104744235A (en) * | 2015-02-28 | 2015-07-01 | 陈学沛 | Process for preparing alpha-linolenic acid |
| CN104719891A (en) * | 2015-03-05 | 2015-06-24 | 陈学沛 | Health product capable of improving immunity |
| CN105341929A (en) * | 2015-12-02 | 2016-02-24 | 烟台燕园科玛健康产业有限公司 | Health-care food composition capable of alleviating asthenopia |
| CN105695093A (en) * | 2016-02-14 | 2016-06-22 | 青海福来喜得生物科技股份有限公司 | Method for extracting high-purity flaxseed oil by aid of molecular distillation processes |
| CN105831766A (en) * | 2016-03-25 | 2016-08-10 | 江苏自然之道生物科技有限公司 | Blood-fat-reducing product and preparation method thereof |
| CN108753455A (en) * | 2018-07-20 | 2018-11-06 | 广州利众生物科技有限公司 | A method of extracting high-purity linseed oil using molecularly distilled |
| CN110157541A (en) * | 2019-05-23 | 2019-08-23 | 河南农业大学 | A kind of woody alpha-linolenic acid concentrated method |
| CN114381333A (en) * | 2020-10-20 | 2022-04-22 | 云南汉盟制药有限公司 | Preparation method of hemp seed oil with high polyunsaturated fatty acid content |
| CN114381333B (en) * | 2020-10-20 | 2023-11-17 | 云南汉盟制药有限公司 | Preparation method of hemp seed oil with high polyunsaturated fatty acid content |
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Application publication date: 20130814 |