CN102329357A - Method for preparing epimedin C - Google Patents
Method for preparing epimedin C Download PDFInfo
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- CN102329357A CN102329357A CN201110210646A CN201110210646A CN102329357A CN 102329357 A CN102329357 A CN 102329357A CN 201110210646 A CN201110210646 A CN 201110210646A CN 201110210646 A CN201110210646 A CN 201110210646A CN 102329357 A CN102329357 A CN 102329357A
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Abstract
The invention relates to a method for preparing epimedin C. The method comprises the following steps of: firstly, by taking Epimedium wushanense T.S.Ying as a raw material, crushing, carrying out microwave extraction by adding 70-90 percent of methanol aqueous solution, decolorizing by adding activated carbon in an extracted solution, depressurizing and concentrating a decolorized liquid to be alcohol-free, deconcentrating by adding water, absorbing by adding a polyamide resin, carrying out gradient elution through a methanol aqueous solution, collecting target components, depressurizing, concentrating, setting and precipitating, removing precipitates, and drying a concentrated liquid to obtain crude extracts; and secondly, separating the crude extracts by adopting a high-speed countercurrent chromatography to obtain high-purity epimedin C. The method provided by the invention has the advantages of simple process, easiness in operation, high product yield rate, high purity and suitability for industrial preparation.
Description
Technical field
The present invention relates to a kind of method for preparing epimedin, particularly relate to a kind of method of utilizing high-speed countercurrent chromatography to prepare epimedin.
Background technology
Epimedin (Epimedin C), flavonoid glycoside compound, fusing point 179-180 ℃ (methyl alcohol), molecular formula C
39H
50O
19, molecular weight 822.8, molecular structural formula:
Epimedin has remarkable increase cell matrix calcium, promotes osteocyte propagation and increases the effect of mineralising tubercle calcium, also has significant immunologic enhancement simultaneously.
Traditional medicine is thought Herba Epimedii property acrid-sweet flavor, temperature, the effect of kidney invigorating and YANG supporting is arranged, dispelling rheumatism.Modern medical research shows that Epimedium contains a lot of flavonoids, with enhanced secretory function of the endocrine system, hormone-like effect, promoting protein synthesis, regulation of cell metabolism, enhance immune function, anti-aging, blood pressure, anti-platelet aggregation, anti-inflammatory , antibacterial, antiviral, expectorant, antitussive, hypoglycemic and hormone-like effects and other pharmacological effects.But Herba Epimedii is divided into bark of a cork tree section plant Herba Epimedii again
Epimedium brevicornumMaxim., arrow leaf Herba Epimedii
Epimedium sagittatum(Sieb.et Zucc.) Maxim., pubescence Herba Epimedii
Epimedium pubescensMaxim., Epimedium wushanense
Epimedium wushanenseT.S.Ying and Herba Epimedii
Epimedium koreanumNaka, epimedin content difference great disparity wherein, Epimedium wushanense content is the highest, in " Chinese Pharmacopoeia-2010 edition ", stipulates the index property composition of epimedin as Epimedium wushanense simultaneously.
Because the epimedin crystallization is difficult, the technology of purifying high-content epimedin is comparatively loaded down with trivial details, and preparation amount is less.Like patent (application number 200610201222.5) " preparation method of epimedin reference substance and products thereof "; This patent disclosed method is the 45-90% alcohol reflux; After extracting solution concentrates; Use sherwood oil, chloroform, ETHYLE ACETATE and n-butanol extraction successively, carry out silicagel column again and separate with polymeric amide.Patent (application number 200710002610.5) " preparation method of epimedin standard reference material "; This patent disclosed method is an alcohol reflux; ETHYLE ACETATE and ETHYLE ACETATE-methanol extraction, extract adopt reverse phase silica gel to separate with gel column after separating with silicagel column again.Also have patent (200810229887.6) " a kind of method for separating and preparing of epimedin chemical reference substance ", the method that this patent adopts is that two steps preparation liquid phase separation obtains product.
Summary of the invention
The objective of the invention is provides a kind of method for preparing epimedin in order to overcome the deficiency of prior art, uses the high speed adverse current chromatogram separation and purification, simple to operate, with short production cycle.
For realizing above-mentioned purpose, technical solution of the present invention is following:
A kind of method for preparing epimedin is characterized in that may further comprise the steps:
1) with the Epimedium wushanense be raw material, pulverize adding 70-90% methanol solution microwave extraction, extracting solution adds activated carbon decolorizing; Destainer is evaporated to no alcohol and adds water-dispersion, adds polyamide resin absorption, the methanol aqueous solution gradient elution; Collect target component, concentrating under reduced pressure is placed deposition; Remove throw out, liquid concentrator is dry, gets crude extract;
2) above-mentioned crude extract adopts high speed adverse current chromatogram to separate, and promptly gets the high purity epimedin.
The optional pharmaceutical powder shaped activated carbon of gac in the step 1), consumption is the 1-2% of amount of liquid.
The described methanol solution gradient elution of step 1) is: 4-5BV20-30% methanol-eluted fractions impurity, 4-5BV40-60% methanol-eluted fractions effective constituent.
Step 2) solvent systems of described high speed adverse current chromatogram is chloroform, methyl alcohol, water, blending ratio 4-5:5-7:3, and getting is moving phase mutually, is stationary phase mutually down.
Step 2) described high speed adverse current chromatogram separation condition is: flow rate of mobile phase 1-3ml/min, and engine speed 700-1000rpm, normal temperature separates, and detector detects wavelength 270nm.
Advantage of the present invention is to adopt high speed adverse current chromatogram to separate, and is liquid liquid distribution chromatography, and the sepn process sample does not lose, and does not produce waste yet, and preparation cycle is short, and preparation amount is big, and product content is high.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1:
Get Epimedium wushanense, get 1kg, add 10 times of amount 70% methanol solution microwave extraction 1 hour, leach liquid; Add 6 times of amount methanol solutions again, microwave extraction 1 hour, extracting solution merges and adds 80 ℃ of decolourings of 2% medicinal carbon 1 hour, filtering gac concentrating under reduced pressure; Liquid concentrator adds water-dispersion, adds polyamide resin column absorption, gets 5BV20% methanol solution wash-out impurity earlier, gets 5BV40% methanol solution wash-out again; Collecting concentrating under reduced pressure does not have alcohol, places deposition, and it is dry to leach the deposition reconcentration, obtains the 18g bullion.Get chloroform, methyl alcohol, water, 5:7:3 mixes in proportion, behind the standing demix, takes off and injects the chromatotube phase that fixes mutually, opens main frame; Adjustment rotating speed 700rpm pumps into phase, after the balance, and adjustment flow velocity 2ml/min; Last phased soln bullion filters the back sample introduction, and UV-detector detects at wavelength 270nm, collects flow point and reclaims reagent; Preparation is drying to obtain epimedin 5.2g continuously, detects content 98.7% through HPLC.
Embodiment 2:
Get Epimedium wushanense, get 1kg, add 6 times of amount 90% methanol solution microwave extraction 30 minutes, extract 3 times; Extracting solution merges and adds 80 ℃ of decolourings of 1% medicinal carbon 1 hour, filtering gac concentrating under reduced pressure, and liquid concentrator adds water-dispersion, adds polyamide resin column absorption; Get 4BV30% methanol solution wash-out impurity earlier, get 4BV60% methanol solution wash-out again, collect concentrating under reduced pressure and do not have alcohol; Place deposition, it is dry to leach the deposition reconcentration, obtains the 15g bullion.Get chloroform, methyl alcohol, water, 4:5:3 mixes in proportion, behind the standing demix, takes off and injects the chromatotube phase that fixes mutually, opens main frame; Adjustment rotating speed 1000rpm pumps into phase, after the balance, and adjustment flow velocity 1ml/min; Last phased soln bullion filters the back sample introduction, and UV-detector detects at wavelength 270nm, collects flow point and reclaims reagent; Preparation is drying to obtain epimedin 4.2g continuously, detects content 98.1% through HPLC.
Embodiment 3:
Get Epimedium wushanense, get 1kg, add 10 times of amount 80% methanol solution microwave extraction 1 hour, leach liquid; Add 6 times of amount methanol solutions again, microwave extraction 1 hour, extracting solution merges and adds 80 ℃ of decolourings of 2% medicinal carbon 1 hour, filtering gac concentrating under reduced pressure; Liquid concentrator adds water-dispersion, adds polyamide resin column absorption, gets 5BV30% methanol solution wash-out impurity earlier, gets 5BV50% methanol solution wash-out again; Collecting concentrating under reduced pressure does not have alcohol, places deposition, and it is dry to leach the deposition reconcentration, obtains the 13g bullion.Get chloroform, methyl alcohol, water, 5:5:3 mixes in proportion, behind the standing demix, takes off and injects the chromatotube phase that fixes mutually, opens main frame; Adjustment rotating speed 800rpm pumps into phase, after the balance, and adjustment flow velocity 3ml/min; Last phased soln bullion filters the back sample introduction, and UV-detector detects at wavelength 270nm, collects flow point and reclaims reagent; Preparation is drying to obtain epimedin 4.5g continuously, detects content 98.4% through HPLC.
Claims (4)
1. method for preparing epimedin is characterized in that may further comprise the steps:
1) with the Epimedium wushanense is raw material, pulverizes that add 70-90% methanol solution microwave extraction, extracting solution adds activated carbon decolorizing; Destainer is evaporated to no alcohol and adds water-dispersion, adds polyamide resin absorption, the methanol aqueous solution gradient elution; Collect target component, concentrating under reduced pressure is placed deposition; Remove throw out, liquid concentrator is dry, gets crude extract;
2) above-mentioned crude extract adopts high speed adverse current chromatogram to separate, and promptly gets the high purity epimedin.
2. according to the said method for preparing epimedin of claim 1, it is characterized in that the described methanol solution gradient elution of step 1) is: 4-5BV20-30% methanol-eluted fractions impurity, 4-5BV40-60% methanol-eluted fractions effective constituent.
3. according to the said method for preparing epimedin of claim 1, it is characterized in that step 2) solvent systems of described high speed adverse current chromatogram is chloroform, methyl alcohol, water, blending ratio 4-5:5-7:3 gets and is moving phase mutually, is stationary phase mutually down.
4. according to the said method for preparing epimedin of claim 1, it is characterized in that step 2) described high speed adverse current chromatogram separation condition is: flow rate of mobile phase 1-3ml/min, engine speed 700-1000rpm, normal temperature separates, and detector detects wavelength 270nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110210646A CN102329357A (en) | 2011-07-26 | 2011-07-26 | Method for preparing epimedin C |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110210646A CN102329357A (en) | 2011-07-26 | 2011-07-26 | Method for preparing epimedin C |
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| CN102329357A true CN102329357A (en) | 2012-01-25 |
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| CN201110210646A Pending CN102329357A (en) | 2011-07-26 | 2011-07-26 | Method for preparing epimedin C |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111848709A (en) * | 2020-07-29 | 2020-10-30 | 劲牌持正堂药业有限公司 | Novel isopentene-based flavonoid compound and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008089669A1 (en) * | 2007-01-23 | 2008-07-31 | Tongjitang Chinese Medicines Company | A novel combination of epimedium-derived-flavonoids-fractions for prevention of steroid-induced osteonecrosis |
| CN101747392A (en) * | 2008-12-17 | 2010-06-23 | 中国科学院大连化学物理研究所 | Method for separating and preparing Cepimedin C chemical reference substance |
| CN101891782A (en) * | 2010-06-23 | 2010-11-24 | 吉林大学 | Separating method of icariside I monomer in Korean epimedium leaves |
| CN102050854A (en) * | 2009-11-10 | 2011-05-11 | 董根荣 | Preparation method and product of epimedin C |
-
2011
- 2011-07-26 CN CN201110210646A patent/CN102329357A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008089669A1 (en) * | 2007-01-23 | 2008-07-31 | Tongjitang Chinese Medicines Company | A novel combination of epimedium-derived-flavonoids-fractions for prevention of steroid-induced osteonecrosis |
| CN101747392A (en) * | 2008-12-17 | 2010-06-23 | 中国科学院大连化学物理研究所 | Method for separating and preparing Cepimedin C chemical reference substance |
| CN102050854A (en) * | 2009-11-10 | 2011-05-11 | 董根荣 | Preparation method and product of epimedin C |
| CN101891782A (en) * | 2010-06-23 | 2010-11-24 | 吉林大学 | Separating method of icariside I monomer in Korean epimedium leaves |
Non-Patent Citations (1)
| Title |
|---|
| HUA-BIN LI: "Separation and Purification of Epimedin A、 B、 C、and Icariin from the Medicinal Herb Epimedium brevicornum Maxim by Dual-Mode HSCCC", 《JOURNAL OF CHROMATOGRAPHIC SCIENCE》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111848709A (en) * | 2020-07-29 | 2020-10-30 | 劲牌持正堂药业有限公司 | Novel isopentene-based flavonoid compound and preparation method and application thereof |
| CN111848709B (en) * | 2020-07-29 | 2022-08-02 | 劲牌持正堂药业有限公司 | Novel isopentene-based flavonoid compound and preparation method and application thereof |
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Application publication date: 20120125 |