CN101070314A - Process for preparing high-purity deoxyschizandrin - Google Patents
Process for preparing high-purity deoxyschizandrin Download PDFInfo
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- CN101070314A CN101070314A CN 200610016838 CN200610016838A CN101070314A CN 101070314 A CN101070314 A CN 101070314A CN 200610016838 CN200610016838 CN 200610016838 CN 200610016838 A CN200610016838 A CN 200610016838A CN 101070314 A CN101070314 A CN 101070314A
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Abstract
This invention relates to a method of preparing high-purity Schisandrin B. The invention adopts analysis mode high speed counter-current chromatography to proceed small scale preparation, adopt semipreparative type high speed counter-current chromatography to proceed large-scale preparation. The feature is that in solvent system the volume ratio of normal hexane, methanol, water and acetonitrile is 5 - 11 : 3 - 6 : 2 - 5 : 1, and the best volume ratio is 10:5:4:3. The invention does not need solid padding, has no irreversible adsorption and no pollution.The purity of gained Schisandrin B can reach 98%upwards.
Description
Technical field:
The present invention relates to a kind of method for preparing high-purity deoxyschizandrin, use high speed adverse current chromatogram (HSCCC) method prepares high-purity deoxyschizandrin from Schisandra chinensis fruit crude extract method.
Background technology:
Schisandra chinensis [Schisandra chinensis (Turcz.) Baill] is the perennial bejuco of Magnoliaceae.Fruit medicine, root and stem rattan also can be used as medicine.Have astringe the lung, nourshing kidney, hidroschesis, promote the production of body fluid, the function of antidiarrheal, puckery essence.Cure mainly cough breathe heavily, body fluid deficiency is thirsty, spontaneous sweating, seminal emission, rush down for a long time, neurasthenia.The recent studies proof also has blood pressure regulation, protects the liver and the effect of " adaptogen " sample.It is a kind of genuine northern rare medicinal herbs.Wuweizisu B is the shizandra berry main active ingredient.Chang Yiqi content still is the significant composition of shizandra berry and goods finger printing thereof as quality control index simultaneously in the goods that with the shizandra berry are main raw material.Therefore say that high-purity deoxyschizandrin is of many uses, demand is big.Bao Dao Wuweizisu B extraction separation mainly was to adopt column chromatography in the past, needed to use solid packing, easily produced irreversible adsorption, had that sample easily loses, easily pollution, poor efficiency, a shortcoming such as speed is slow and separating step is loaded down with trivial details.
Summary of the invention:
The object of the present invention is to provide a kind of method for preparing high-purity deoxyschizandrin, is to use high speed adverse current chromatogram (HSCCC) method to prepare high-purity deoxyschizandrin from the shizandra berry crude extract; It need not use solid packing, carries out the separation and purification of natural product but use under the mode of the immiscible solvent systems high speed planetary motion in supporting tube of two-phase, thereby does not have irreversible adsorption; Have sample free of losses, the isolating advantage of pollution-free, efficient, quick and big preparation amount.
The technical scheme of this invention is achieved in that a kind of method for preparing high-purity deoxyschizandrin, adopt a small amount of preparation of analysis mode high-speed counter-current chromatograph and the relatively large preparation of half countercurrent chromatography instrument, it is characterized in that: with normal hexane-methanol-water-acetonitrile volume ratio is the solvent systems of 5-11: 3-6: 2-5: 1-4, and normal hexane-methanol-water-acetonitrile optimum volume ratio is 10: 5: 4: 3 carry out flash liberation makes Wuweizisu B.
Room temperature has certain influence to resolution, and above separation condition is fit to room temperature and uses in the time of 16-28 ℃.When room temperature reduces, reduce the ratio of methyl alcohol, to improve resolution.Vice versa.
Positively effect of the present invention is: provide a kind of and need not use solid packing, do not had irreversible adsorption, the method that sample free of losses, pollution-free, efficient, quick, low-cost and big preparation amount separate Wuweizisu B.
Embodiment:
The present invention will be further described below in conjunction with embodiment:
Embodiment 1:
Adopt the analysis mode high-speed counter-current chromatograph, solvent is selected normal hexane-methanol-water-acetonitrile system for use.At first with 6: 3: 3: 1 volume ratio places separating funnel with above-mentioned solvent system, shakes up the back static layering.Ready to balance separates upper and lower phase after for some time, more than be stationary phase mutually, is moving phase mutually down.It is stand-by in being dissolved under the 2ml mutually to get an amount of shizandra berry crude extract.Adopt the U.S. to produce CCC-3000 type high-speed counter-current chromatograph and separate, stationary phase is filled with chromatography column, the opening speed controller, when reaching desired speed, beginning pumps into moving phase with certain flow rate, when moving phase flows out, by the six-way injection valve sample introduction.By head end wash-out caudad, main frame just changes, and rotating speed is 1300r/min, regularly collects component.
Embodiment 2:
Adopt half countercurrent chromatography instrument, solvent is selected normal hexane-methanol-water-acetonitrile system for use.At first with 9: 4: 3: 2 volume ratios place separating funnel with above-mentioned solvent system, shake up the back static layering.Ready to balance separates upper and lower phase after for some time, more than be stationary phase mutually, is moving phase mutually down.It is stand-by in being dissolved under the 10ml mutually to get an amount of shizandra berry crude extract.Adopt the U.S. to produce CCC-1000 type high-speed counter-current chromatograph and separate, stationary phase is filled with chromatography column, the opening speed controller, when reaching desired speed, beginning pumps into moving phase with certain flow rate, when moving phase flows out, by the six-way injection valve sample introduction.By head end wash-out caudad, main frame just changes, and rotating speed is 900r/min, regularly collects component.
Embodiment 3:
Adopt the analysis mode high-speed counter-current chromatograph, solvent is selected normal hexane-methanol-water-acetonitrile system for use.At first with 5: 3: 2: 1 volume ratio places separating funnel with above-mentioned solvent system, shakes up the back static layering.Ready to balance separates upper and lower phase after for some time, more than be stationary phase mutually, is moving phase mutually down.It is stand-by in being dissolved under the 2ml mutually to get an amount of shizandra berry crude extract.Adopt the U.S. to produce CCC-3000 type high-speed counter-current chromatograph and separate, stationary phase is filled with chromatography column, the opening speed controller, when reaching desired speed, beginning pumps into moving phase with certain flow rate, when moving phase flows out, by the six-way injection valve sample introduction.By head end wash-out caudad, main frame just changes, and rotating speed is 1300r/min, regularly collects component.
Embodiment 4:
Adopt the analysis mode high-speed counter-current chromatograph, solvent is selected normal hexane-methanol-water-acetonitrile system for use.At first with 11: 6: 5: 4 volume ratios place separating funnel with above-mentioned solvent system, shake up the back static layering.Ready to balance separates upper and lower phase after for some time, more than be stationary phase mutually, is moving phase mutually down.It is stand-by in being dissolved under the 10ml mutually to get an amount of shizandra berry crude extract.Adopt the U.S. to produce CCC-3000 type high-speed counter-current chromatograph and separate, stationary phase is filled with chromatography column, the opening speed controller, when reaching desired speed, beginning pumps into moving phase with certain flow rate, when moving phase flows out, by the six-way injection valve sample introduction.By head end wash-out caudad, main frame just changes, and rotating speed is 900r/min, regularly collects component.
Claims (2)
1, a kind of method for preparing high-purity deoxyschizandrin, it is characterized in that: adopt a small amount of preparation of analysis mode high-speed counter-current chromatograph and the relatively large preparation of half countercurrent chromatography instrument, with normal hexane-methanol-water-acetonitrile volume ratio is the solvent systems of 5-11: 3-6: 2-5: 1-4, carries out flash liberation and makes Wuweizisu B.
2, a kind of method for preparing high-purity deoxyschizandrin according to claim 1 is characterized in that described solvent systems normal hexane-methanol-water-acetonitrile optimum volume ratio is 10: 5: 4: 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610016838 CN101070314A (en) | 2006-05-10 | 2006-05-10 | Process for preparing high-purity deoxyschizandrin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200610016838 CN101070314A (en) | 2006-05-10 | 2006-05-10 | Process for preparing high-purity deoxyschizandrin |
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| CN101070314A true CN101070314A (en) | 2007-11-14 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050707A (en) * | 2009-11-01 | 2011-05-11 | 桂林莱茵生物科技股份有限公司 | Method for extracting deoxyschisandrin and schisandrin B from schisandra |
| CN101709059B (en) * | 2009-12-09 | 2012-09-26 | 北京博远欣绿科技有限公司 | Chinese magnoliavine fruit monomer composition separation preparation method |
| CN103351373A (en) * | 2013-05-31 | 2013-10-16 | 浙江鼎辉医药科技有限公司 | Method for extracting Schisandrin B from Schisandra chinensis |
| CN103467438A (en) * | 2013-09-18 | 2013-12-25 | 浙江工业大学 | Method for extracting, separating and preparing lignin monomers from schisandra chinensis |
-
2006
- 2006-05-10 CN CN 200610016838 patent/CN101070314A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102050707A (en) * | 2009-11-01 | 2011-05-11 | 桂林莱茵生物科技股份有限公司 | Method for extracting deoxyschisandrin and schisandrin B from schisandra |
| CN101709059B (en) * | 2009-12-09 | 2012-09-26 | 北京博远欣绿科技有限公司 | Chinese magnoliavine fruit monomer composition separation preparation method |
| CN103351373A (en) * | 2013-05-31 | 2013-10-16 | 浙江鼎辉医药科技有限公司 | Method for extracting Schisandrin B from Schisandra chinensis |
| CN103351373B (en) * | 2013-05-31 | 2014-11-05 | 浙江鼎辉医药科技有限公司 | Method for extracting Schisandrin B from Schisandra chinensis |
| CN103467438A (en) * | 2013-09-18 | 2013-12-25 | 浙江工业大学 | Method for extracting, separating and preparing lignin monomers from schisandra chinensis |
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Open date: 20071114 |