CN101607976A - A kind of preparation method of icarin - Google Patents
A kind of preparation method of icarin Download PDFInfo
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- CN101607976A CN101607976A CNA2008101290152A CN200810129015A CN101607976A CN 101607976 A CN101607976 A CN 101607976A CN A2008101290152 A CNA2008101290152 A CN A2008101290152A CN 200810129015 A CN200810129015 A CN 200810129015A CN 101607976 A CN101607976 A CN 101607976A
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Abstract
The invention provides a kind of preparation method of icarin, get epimedium herb,, reclaim solvent, be condensed into medicinal extract with methyl alcohol or the alcohol reflux of 30-90%; Be extracted to closely colourlessly successively with sherwood oil, chloroform, ethyl acetate and propyl carbinol repeatedly, reclaim propyl carbinol to doing, crude extract; Carry out the silica gel column chromatography separation then successively and separate, promptly get the icarin highly finished product, purity 〉=98% with polyamide column chromatography.Compared with prior art, the invention provides a kind of less column chromatography that only needs, the yield higher purity is the icarin extracting and preparing technique more than 98%.
Description
Technical field:
The present invention relates to a kind of preparation method of icarin, belong to the extractive technique field of index components in the medicinal material.
Background technology:
Herba Epimedii is the conventional Chinese medicine that the Pharmacopoeia of the People's Republic of China records, and has the effect of kidney-replenishing, strengthening the bones and muscles, wind-damp dispelling, is mainly used in impotence and seminal emission, and muscles and bones is soft repeatly, rheumatic arthralgia, numbness contracture, diseases such as climacteric hypertension.The contained total flavonoid composition of Herba Epimedii is one of efficient part, comprise multiple flavones ingredients such as icarin, icariside, wherein icarin is the main medicinal ingredients in epimedium herb and the preparation, have the cardiovascular and cerebrovascular of increasing volume of blood flow, enhancing antibody generation, promote that DNA is synthetic, reach androgen-like action, can promote hemopoietic function, immunologic function and bone metabolism, have effects such as anti-ageing, antitumor.For a long time, domestic and international experts and scholars have invented the extracting method of a lot of icarin.Compared with prior art, the invention provides a kind of less column chromatography that only needs, the yield higher purity is the icarin extracting and preparing technique more than 98%.
Summary of the invention:
The objective of the invention is to: the preparation method that a kind of icarin is provided.The present invention investigates by the extraction process to epimedium herb comprehensively, has determined the optimum extraction process of icarin, and successfully icarin has been carried out separation and purifying.
The present invention is achieved in that the preparation method of icarin is: extract (1): get epimedium herb, be cut into disconnectedly, add 10-40 and doubly measure the methyl alcohol of 30-90% or alcohol reflux 2-5 time, each 0.5-2h merges all extracting solutions, reclaims solvent, must fluid extract; The fluid extract adding distil water is placed in right amount, abandons precipitation, gets supernatant liquor, and reconcentration gets concentrated extract; Use sherwood oil, chloroform, ethyl acetate extraction to closely colourless successively, be extracted to closely colourlessly again with propyl carbinol repeatedly, reclaim propyl carbinol, promptly get the crude extract that contains icarin to doing; (2) separate: contain the icarin crude extract with dissolve with methanol, the thin-layer chromatography silica gel mixed sample, silica gel column chromatography separates, with chloroform: methyl alcohol=100: 8, carried out gradient elution in 100: 13,100: 17,100: 20,100: 22, following the tracks of inspection with the silica gel precoated plate knows, Rf value Rf equals spot stream part of icarin reference substance on the prefabricated thin-layer chromatography TLC of the collection silica gel plate, behind the recovery solvent, promptly gets the icarin crude product; The crude product dissolve with methanol, column chromatography is mixed sample with polymeric amide, polyamide column chromatography separates, with ethyl acetate: ethanol: water=8: 0: 0, carried out gradient elution in 8: 0.5: 0,8: 1: 0.1,8: 1: 0.2, examine knowledge with the polyamide layer tracking, Rf value Rf equals spot stream part of icarin reference substance on the collection polyamide layer thin-layer chromatography TLC plate, can obtain the icarin highly finished product behind the recovery solvent, place moisture eliminator more than 24 hours, promptly get the icarin of purity 〉=98%.
Better leaching process is: get epimedium herb, be cut into disconnectedly, add 20 times of amounts 70% methyl alcohol or alcohol refluxs 3 times, each 1h merges three times extracting solution, reclaims solvent, must fluid extract; The fluid extract adding distil water is placed in right amount, abandons precipitation, gets supernatant liquor, and reconcentration gets concentrated extract; Use sherwood oil, chloroform, ethyl acetate extraction to closely colourless successively, be extracted to closely colourlessly again with propyl carbinol repeatedly, reclaim propyl carbinol, promptly get the crude extract that contains icarin to doing.
Wherein the development system of silica gel thin-layer chromatography TLC is a chloroform: methyl alcohol=100: 20.
The development system of polyamide layer thin-layer chromatography TLC is an ethyl acetate: ethanol: water=8: 1: 0.2.
The used raw material Herba Epimedii of above-mentioned preparation method is any in Berberidaceae Epimedium (Epimedium) and America Epimedium (Vancouveria) plant.
The developer that uses silica gel thin-layer chromatography to detect icarin among the preparation method of the present invention is 5% ethanol solution of sulfuric acid, the heating colour developing.
Description of drawings
Figure-1 is the HPLC collection of illustrative plates of icarin product.
Embodiment:
Be embodiments of the invention below, but the present invention is not limited only to described embodiment.
Embodiment 1:
(1) extraction process:
Get epimedium herb, be cut into disconnectedly, add 20 times of 70% methyl alcohol or alcohol reflux 3 times, each 1h merges three times extracting solution, the recovery solvent, and be condensed into fluid extract.The fluid extract adding distil water is placed in right amount, abandons precipitation, gets supernatant liquor, and reconcentration gets medicinal extract.Use sherwood oil, chloroform, ethyl acetate extraction to closely colourless successively, be extracted to closely colourlessly again with propyl carbinol repeatedly, reclaim propyl carbinol, promptly obtain containing the crude extract of icarin to doing.
(2) separating technology:
1. the separation of silica gel column chromatography:
With above-mentioned gained crude extract dissolve with methanol, the thin-layer chromatography silica gel mixed sample, silica gel column chromatography separates, with chloroform: methyl alcohol (100: 8,100: 13,100: 17,100: 20,100: 22) gradient elution, follow the tracks of inspection with the silica gel precoated plate and know, development system is a chloroform: methyl alcohol=100: 20, and collect silica gel precoated plate TLC and go up spot stream part that Rf value equals icarin, after reclaiming solvent, promptly get the icarin crude product.
2. the separation of polyamide column chromatography:
Icarin crude product dissolve with methanol, column chromatography is mixed sample with polymeric amide, polyamide column chromatography separates, with ethyl acetate: ethanol: water (8: 0: 0,8: 0.5: 0,8: 1: 0.1,8: 0: 0.2) gradient elution, following the tracks of inspection with polyamide layer knows, development system is an ethyl acetate: ethanol: water=8: 1: 0.2, collect polyamide layer TLC and go up spot stream part that the Rf value equals icarin, can obtain the icarin highly finished product after reclaiming solvent, place moisture eliminator more than 24 hours, promptly get the icarin of purity 〉=98%.
Embodiment 2:
Extraction process: get epimedium herb, be cut into disconnectedly, add 10 times of 90% methyl alcohol or alcohol reflux 2 times, each 2h merges twice extracting solution, recovery solvent, and concentrated fluid extract.The fluid extract adding distil water is placed in right amount, abandons precipitation, gets supernatant liquor, and reconcentration gets medicinal extract.Use sherwood oil, chloroform, ethyl acetate extraction to closely colourless successively, be extracted to closely colourlessly again with propyl carbinol repeatedly, reclaim propyl carbinol, promptly obtain containing the crude extract of icarin to doing.
The separating technology of icarin crude extract is described with embodiment 1.
Embodiment 3:
Extraction process: get epimedium herb, be cut into disconnectedly, add 40 times of 45% methyl alcohol or alcohol reflux 5 times, each 0.5h merges five times extracting solution, the recovery solvent, and be condensed into fluid extract.The fluid extract adding distil water is placed in right amount, abandons precipitation, gets supernatant liquor, and reconcentration gets medicinal extract.Use sherwood oil, chloroform, ethyl acetate extraction to closely colourless successively, be extracted to closely colourlessly again with propyl carbinol repeatedly, reclaim propyl carbinol, promptly obtain containing the crude extract of icarin to doing.
The separating technology of icarin crude extract is described with embodiment 1.
Claims (6)
1: a kind of preparation method of icarin is characterized in that: extract (1): get epimedium herb, be cut into disconnectedly, add 10-40 and doubly measure the methyl alcohol of 30-90% or alcohol reflux 2-5 time, each 0.5-2h merges all extracting solutions, reclaims solvent, must fluid extract; The fluid extract adding distil water is placed in right amount, abandons precipitation, gets supernatant liquor, and reconcentration gets concentrated extract; Use sherwood oil, chloroform, ethyl acetate extraction to closely colourless successively, be extracted to closely colourlessly again with propyl carbinol repeatedly, reclaim propyl carbinol, promptly get the crude extract that contains icarin to doing.(2) separate: contain the icarin crude extract with dissolve with methanol, the thin-layer chromatography silica gel mixed sample, silica gel column chromatography separates, with chloroform: methyl alcohol=100: 8, carried out gradient elution in 100: 13,100: 17,100: 20,100: 22, following the tracks of inspection with the silica gel precoated plate knows, Rf value Rf equals spot stream part of icarin reference substance on the prefabricated thin-layer chromatography TLC of the collection silica gel plate, behind the recovery solvent, promptly gets the icarin crude product; The crude product dissolve with methanol, column chromatography is mixed sample with polymeric amide, polyamide column chromatography separates, with ethyl acetate: ethanol: water=8: 0: 0, carried out gradient elution in 8: 0.5: 0,8: 1: 0.1,8: 1: 0.2, examine knowledge with the polyamide layer tracking, Rf value Rf equals spot stream part of icarin reference substance on the collection polyamide layer thin-layer chromatography TLC plate, can obtain the icarin highly finished product behind the recovery solvent, place moisture eliminator more than 24 hours, promptly get the icarin of purity 〉=98%.
2: the preparation method according to the described icarin of claim 1 is characterized in that: described leaching process is: get epimedium herb, be cut into disconnected, add 20 times of amount 70% methyl alcohol or alcohol reflux 3 times, each 1h merges three times extracting solution, reclaim solvent, get fluid extract; The fluid extract adding distil water is placed in right amount, abandons precipitation, gets supernatant liquor, and reconcentration gets medicinal extract; Use sherwood oil, chloroform, ethyl acetate extraction to closely colourless successively, be extracted to closely colourlessly again with propyl carbinol repeatedly, reclaim propyl carbinol and contain the icarin crude extract to doing, promptly getting.
3: the preparation method according to the described icarin of claim 1 is characterized in that: the development system of silica gel thin-layer chromatography TLC is a chloroform: methyl alcohol=100: 20.
4: the preparation method according to the described icarin of claim 1 is characterized in that: the development system of polyamide layer thin-layer chromatography TLC is an ethyl acetate: ethanol: water=8: 1: 0.2.
5: by the preparation method of the described icarin of claim 1, it is characterized in that: used raw material Herba Epimedii is any in Berberidaceae Epimedium (Epimedium) and America Epimedium (Vancouveria) plant.
6: the preparation method by the described icarin of claim 1 is characterized in that: the developer in the silica gel thin-layer chromatography in the method for detection icarin is 5% ethanol solution of sulfuric acid, the heating colour developing.
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| CN 200810129015 CN101607976B (en) | 2008-06-19 | 2008-06-19 | Method for preparing icariin |
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| CN 200810129015 CN101607976B (en) | 2008-06-19 | 2008-06-19 | Method for preparing icariin |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812100A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Method for preparing icariin |
| CN102617670A (en) * | 2011-01-27 | 2012-08-01 | 北京市理化分析测试中心 | Preparation method of icariin monomer |
| CN102807595A (en) * | 2011-06-02 | 2012-12-05 | 汉中天然谷生物科技有限公司 | Technique for preparing high-content (98 percent) icariin from Epimedium plant |
| CN103288901A (en) * | 2013-05-13 | 2013-09-11 | 张洋 | Preparation process of epimedium extractive |
| CN103396463A (en) * | 2013-08-22 | 2013-11-20 | 内蒙古鑫吉利生物科技有限公司 | Method for extracting icariin from epimedium |
| CN105925635A (en) * | 2016-05-04 | 2016-09-07 | 宁波旋光医药科技有限公司 | Production process of icariside II |
| CN106589020A (en) * | 2016-12-31 | 2017-04-26 | 北京颐方生物科技有限公司 | Method for extracting icariin from epimedium |
| CN107496490A (en) * | 2017-09-25 | 2017-12-22 | 安徽金源药业有限公司 | One kind extraction glycoside substance method |
| CN109771465A (en) * | 2018-12-28 | 2019-05-21 | 广州中医药大学(广州中医药研究院) | It is a kind of to be combined with the effective ingredient in Chinese for significantly inhibiting HIV/SIV effect |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6294476B2 (en) | 2013-10-21 | 2018-03-14 | ▲魯▼南制▲薬▼集▲団▼股▲フン▼有限公司 | Use of anhydroicaritin in the manufacture of a medicament for preventing or treating cytopenias |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101812100A (en) * | 2010-04-08 | 2010-08-25 | 苏州宝泽堂医药科技有限公司 | Method for preparing icariin |
| CN102617670A (en) * | 2011-01-27 | 2012-08-01 | 北京市理化分析测试中心 | Preparation method of icariin monomer |
| CN102807595A (en) * | 2011-06-02 | 2012-12-05 | 汉中天然谷生物科技有限公司 | Technique for preparing high-content (98 percent) icariin from Epimedium plant |
| CN103288901A (en) * | 2013-05-13 | 2013-09-11 | 张洋 | Preparation process of epimedium extractive |
| CN103396463A (en) * | 2013-08-22 | 2013-11-20 | 内蒙古鑫吉利生物科技有限公司 | Method for extracting icariin from epimedium |
| CN103396463B (en) * | 2013-08-22 | 2016-05-18 | 内蒙古鑫吉利生物科技有限公司 | A kind of method of extracting icariin from barrenwort |
| CN105925635A (en) * | 2016-05-04 | 2016-09-07 | 宁波旋光医药科技有限公司 | Production process of icariside II |
| CN106589020A (en) * | 2016-12-31 | 2017-04-26 | 北京颐方生物科技有限公司 | Method for extracting icariin from epimedium |
| CN106589020B (en) * | 2016-12-31 | 2019-03-22 | 北京颐方生物科技有限公司 | A method of extracting icariin from Herba Epimedii |
| CN107496490A (en) * | 2017-09-25 | 2017-12-22 | 安徽金源药业有限公司 | One kind extraction glycoside substance method |
| CN108976264A (en) * | 2017-09-25 | 2018-12-11 | 安徽金源药业有限公司 | A kind of kidney tonifying, benefiting essence-blood, radiation protection saussurea involucrata Herba Epimedii root of kirilow rhodiola Chinese medicine composition |
| CN109771465A (en) * | 2018-12-28 | 2019-05-21 | 广州中医药大学(广州中医药研究院) | It is a kind of to be combined with the effective ingredient in Chinese for significantly inhibiting HIV/SIV effect |
| CN109771465B (en) * | 2018-12-28 | 2021-04-27 | 广州中医药大学(广州中医药研究院) | Traditional Chinese medicine effective part composition with significant HIV/SIV inhibition effect |
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