CN107176909A - A kind of method that use supercritical fluid chromatography purifies docosahexaenoic acid - Google Patents
A kind of method that use supercritical fluid chromatography purifies docosahexaenoic acid Download PDFInfo
- Publication number
- CN107176909A CN107176909A CN201610135297.1A CN201610135297A CN107176909A CN 107176909 A CN107176909 A CN 107176909A CN 201610135297 A CN201610135297 A CN 201610135297A CN 107176909 A CN107176909 A CN 107176909A
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- China
- Prior art keywords
- entrainer
- docosahexaenoic acid
- supercritical fluid
- fluid chromatography
- methanol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses a kind of method that use supercritical fluid chromatography purifies docosahexaenoic acid, stationary phase, supercritical CO are used as using naked silica gel, C18, C8, glycol-based2Mobile phase is done, methanol, ethanol, acetonitrile do entrainer, and purifying obtains more than 99% docosahexaenoic acid.The method does mobile phase using CO2, only adds a small amount of organic solvent, reduces pollution of the organic solvent to environment, environmental protection, meanwhile, preparation process is simple, it is easy to operate.
Description
Technical field
The present invention relates to a kind of purification process of natural products, the particularly purification process of docosahexaenoic acid.
Background technology
Docosahexaenoic acid, English name is Docosahexaenoicacid, English abbreviation DHA, it is a kind of polyunsaturated fatty acid necessary to human body, content is more in fish oil, and the 22 of a kind of straight chain fatty acid, only its n-3 family containing 22 carbon atoms and 6 double bonds:6 Δ 4c, 7c, 10c, 13c, 16c, 19c isomers are largely present in fish oil (account for fatty acid total amount 10%~15%) with native form, the glycerophosphatide of animal then acid containing inequality, in metabolic process, can be generated from alpha linolenic acid.
Supercritical extract is simply introduced：Supercritical CO2Fluid extraction（SFE）The principle of separation process is the relation of solvability and its density using supercritical fluid, the i.e. influence using pressure and temperature to supercritical fluid solvability and carried out.In the supercritical state, supercritical fluid is contacted with material to be separated, makes it that selectively the composition of polarity size, boiling point height and molecular size range be extracted successively.Certainly, extract obtained by each pressure limit of correspondence is unlikely to be single, but the blending constituent of optimal proportion can be obtained with control condition, then supercritical fluid is made to become common gases by the method for decompression, heating, material is extracted then wholly or substantially to separate out, so as to reach the purpose of separating-purifying, so supercritical CO2Fluid extraction process is combined by extraction and separation process.
The content of the invention
The technical solution adopted by the present invention is as follows：Stationary phase, supercritical CO are used as using the silica matrix class filler such as naked silica gel, C18, C8, glycol-based2Do mobile phase, methanol, ethanol, acetonitrile do entrainer, purifying obtains the docosahexaenoic acid that purity is more than 99%, comprises the following steps：
（1）Fish oil crude product, 0.45um filtering with microporous membrane are dissolved using methanol；
（2）Configure methanol：Ethanol：Acetonitrile=2:3:1 entrainer；
（3）Using the flow visualizing balance system 20min of the entrainer of low ratio, then sample introduction starts to collect target components after about 50min, collects after about 10min, reuse a high proportion of entrainer and eluted；
（4）The cut of collection is post-processed using Rotary Evaporators, obtained white powder as target product.
The present invention has following technical advantage：Purified using supercritical fluid chromatography and obtain the docosahexaenoic acid that purity is more than 99%, the method uses CO2Mobile phase is done, a small amount of organic solvent is only added, pollution of the organic solvent to environment is reduced, environmental protection, meanwhile, preparation process is simple, it is easy to operate.
Embodiment
Embodiment 1
Fish oil crude product is dissolved using methanol, 0.45um filtering with microporous membrane configures methanol：Ethanol：Acetonitrile=2:3:1 entrainer, naked silica gel uses supercritical CO as stationary phase2：Entrainer=92:Start to collect target components after 8 flow visualizing balance system 20min, sample introduction, elution about 50min, collect after about 10min, reuse supercritical CO2：Entrainer=8:92 mobile phase is eluted, and the cut of collection is post-processed using Rotary Evaporators, obtained white powder as target product.
Embodiment 2
Fish oil crude product is dissolved using methanol, 0.45um filtering with microporous membrane configures methanol：Ethanol：Acetonitrile=2:3:1 entrainer, C18 silica gel uses supercritical CO as stationary phase2：Entrainer=95:Start to collect target components after 5 flow visualizing balance system 20min, sample introduction, elution about 50min, collect after about 10min, reuse supercritical CO2：Entrainer=5:95 mobile phase is eluted, and the cut of collection is post-processed using Rotary Evaporators, obtained white powder as target product.
Embodiment 3
Fish oil crude product is dissolved using methanol, 0.45um filtering with microporous membrane configures methanol：Ethanol：Acetonitrile=2:3:1 entrainer, C18 silica gel uses supercritical CO as stationary phase2：Entrainer=97:Start to collect target components after 3 flow visualizing balance system 20min, sample introduction, elution about 50min, collect after about 10min, reuse supercritical CO2：Entrainer=3:97 mobile phase is eluted, and the cut of collection is post-processed using Rotary Evaporators, obtained white powder as target product.
Claims (2)
1. a kind of method that use supercritical fluid chromatography purifies docosahexaenoic acid, it is characterised in that：
（1）Fish oil crude product is dissolved using methanol, 0.45um miillpore filter is filtered；
（2）Configure methanol：Ethanol：Acetonitrile=2:3:1 entrainer；
（3）Using the flow visualizing balance system 20min of the entrainer of low ratio, sample introduction elutes and starts to collect target components after about 50min, collects about 10min, reuse a high proportion of entrainer and eluted；
（4）Cut after collection is post-processed using Rotary Evaporators, obtained white powder as target product.
2. the method that a kind of use supercritical fluid chromatography according to claim 1 purifies docosahexaenoic acid, it is characterised in that：Stationary phase, supercritical CO are used as using naked silica gel, C18, C8, glycol-based2Do mobile phase.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610135297.1A CN107176909A (en) | 2016-03-10 | 2016-03-10 | A kind of method that use supercritical fluid chromatography purifies docosahexaenoic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610135297.1A CN107176909A (en) | 2016-03-10 | 2016-03-10 | A kind of method that use supercritical fluid chromatography purifies docosahexaenoic acid |
Publications (1)
| Publication Number | Publication Date |
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| CN107176909A true CN107176909A (en) | 2017-09-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201610135297.1A Withdrawn CN107176909A (en) | 2016-03-10 | 2016-03-10 | A kind of method that use supercritical fluid chromatography purifies docosahexaenoic acid |
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| CN (1) | CN107176909A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113563178A (en) * | 2021-08-27 | 2021-10-29 | 常熟纳微生物科技有限公司 | Method for separating and purifying docosahexaenoic acid in fish oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634852A (en) * | 2004-10-25 | 2005-07-06 | 浙江大学 | Process for preparing and separating eicosapentaenoic acid ethyl ester and docosahexenoic acid ethyl ester |
| CN103804171A (en) * | 2014-02-25 | 2014-05-21 | 国家海洋局第三海洋研究所 | Preparation method and device for polyenoic acid and ester monomer thereof |
-
2016
- 2016-03-10 CN CN201610135297.1A patent/CN107176909A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634852A (en) * | 2004-10-25 | 2005-07-06 | 浙江大学 | Process for preparing and separating eicosapentaenoic acid ethyl ester and docosahexenoic acid ethyl ester |
| CN103804171A (en) * | 2014-02-25 | 2014-05-21 | 国家海洋局第三海洋研究所 | Preparation method and device for polyenoic acid and ester monomer thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113563178A (en) * | 2021-08-27 | 2021-10-29 | 常熟纳微生物科技有限公司 | Method for separating and purifying docosahexaenoic acid in fish oil |
| CN113563178B (en) * | 2021-08-27 | 2024-06-04 | 常熟纳微生物科技有限公司 | Separation and purification method of docosahexaenoic acid in fish oil |
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Application publication date: 20170919 |