CN101070335A - Process for preparing high-purity gentiopicrin - Google Patents
Process for preparing high-purity gentiopicrin Download PDFInfo
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- CN101070335A CN101070335A CN 200610016839 CN200610016839A CN101070335A CN 101070335 A CN101070335 A CN 101070335A CN 200610016839 CN200610016839 CN 200610016839 CN 200610016839 A CN200610016839 A CN 200610016839A CN 101070335 A CN101070335 A CN 101070335A
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- gentiopicrin
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- rough gentian
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Abstract
This invention relates to a method of preparing high-purity gentiopicrin. The invention adopts small scale preparation by analysis mode high speed counter-current chromatography, and large-scale preparation by semipreparing type high speed counter-current chromatography; volume ratio of chloroform, methanol, normal butyl alcohol and water is 4-8:3-6:1-4:3-6; one time separation to gain gentiopicrin. No need solid filling and without irreversible adsorption. The acquired gentiopicrin purity reach 92%upwards, lend itself to prepare gentiopicrin from different kinds of rough gentian crude extract.
Description
Technical field:
The present invention relates to a kind of method for preparing high-purity gentiopicrin, is a kind of application high speed adverse current chromatogram (HSCCC) method prepares high-purity gentiopicrin from the rough gentian crude extract method.
Background technology:
Rough gentian is the dry root and rhizome of gentianaceae plant bar leaf rough gentian Gentiana manshurica Kitag., rough gentian Gentiana scabra Bge., three flower rough gentian Gentiana triflora pall. or hard rough gentian Gentiana rigescens Franch..The main effective constituent of its medicinal part is gentiopicrin, and gentiopicrin belongs to the iridoid glycoside compounds, and the effect of clearing liver detoxifcation, food digesting stomach fortifying is arranged.Gentiopicrin is by 2005 editions quantitative chemical indexs as rough gentian HPLC method assay of Chinese Pharmacopoeia.Still be the significant composition of rough gentian and goods finger printing thereof simultaneously.Therefore say that high-purity gentiopicrin is of many uses, demand is big.Bao Dao gentiopicrin 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 gentiopicrin, is to use high speed adverse current chromatogram (HSCCC) method to prepare high-purity gentiopicrin from the rough gentian crude extract; Be need not use solid packing, but use the separation and purification of carrying out natural product under the mode of the immiscible solvent systems high speed planetary motion in supporting tube of two-phase, thereby do not have irreversible adsorption, have sample free of losses, the isolating advantage of pollution-free, efficient, quick and big preparation amount.
Technical scheme of the present invention is achieved in that a kind of method for preparing high-purity gentiopicrin, 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, selecting chloroform-methanol-n-butanol-water volume ratio for use is the solvent systems of 4-8: 3-6: 1-4: 3-6, and flash liberation can obtain gentiopicrin.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 gentiopicrin.
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 system for use.At first with 4: 5: 3: 5 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 2ml mutually to get an amount of rough gentian 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 system for use.At first with 7: 3: 1: 3 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 rough gentian 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 system for use.At first with 4: 3: 1: 3 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 2ml mutually to get an amount of rough gentian 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 system for use.At first with 8: 6: 4: 6 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 rough gentian 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 (1)
1, a kind of method for preparing high-purity gentiopicrin, it is characterized in that: selecting chloroform-methanol-n-butanol-water volume ratio for use is the solvent systems of 4-8: 3-6: 1-4: 3-6, adopt a small amount of preparation of analysis mode high-speed counter-current chromatograph and the relatively large preparation of half countercurrent chromatography instrument, flash liberation can obtain gentiopicrin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610016839 CN101070335A (en) | 2006-05-10 | 2006-05-10 | Process for preparing high-purity gentiopicrin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610016839 CN101070335A (en) | 2006-05-10 | 2006-05-10 | Process for preparing high-purity gentiopicrin |
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| Publication Number | Publication Date |
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| CN101070335A true CN101070335A (en) | 2007-11-14 |
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| CN 200610016839 Pending CN101070335A (en) | 2006-05-10 | 2006-05-10 | Process for preparing high-purity gentiopicrin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286042A (en) * | 2010-06-17 | 2011-12-21 | 上海中药制药技术有限公司 | Separation preparation method for high-purity phillyrin |
| CN103063798A (en) * | 2013-01-01 | 2013-04-24 | 吉林紫鑫药业股份有限公司 | Novel method for detecting Longdan Xiegan particles |
| CN103848875A (en) * | 2012-11-30 | 2014-06-11 | 哈尔滨誉衡药业股份有限公司 | Preparation method of gentiopicroside raw material |
-
2006
- 2006-05-10 CN CN 200610016839 patent/CN101070335A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102286042A (en) * | 2010-06-17 | 2011-12-21 | 上海中药制药技术有限公司 | Separation preparation method for high-purity phillyrin |
| CN103848875A (en) * | 2012-11-30 | 2014-06-11 | 哈尔滨誉衡药业股份有限公司 | Preparation method of gentiopicroside raw material |
| CN103063798A (en) * | 2013-01-01 | 2013-04-24 | 吉林紫鑫药业股份有限公司 | Novel method for detecting Longdan Xiegan particles |
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Open date: 20071114 |