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Method for separating and purifying gentiamarin

A technology of gentiopicroside and purification method, which is applied in the field of separating high-purity gentiopicroside, can solve the problems of being unsuitable for the preparation and use of a large number of products, the purity is not high enough, and the use restriction, etc. The effect of the amount of extraction

Inactive Publication Date: 2012-09-19
HENAN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Currently reported methods for the separation and purification of gentiopicroside mainly contain two types: one uses macroporous adsorption resin method, which has a large amount of separation, but the purity is not high enough; the other uses high-speed countercurrent chromatography, which uses The amount is small, not suitable for the preparation of a large number of products, and the equipment is expensive, and the use is limited

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The method for separating and purifying gentiopicroside of the present embodiment adopts the following steps:

[0015] 1) Weigh 600 g of 200-mesh column chromatography silica gel, add a mixed solvent of chloroform and methanol with a volume ratio of 9:1, stir until there are no bubbles, pour it into a glass chromatography column, and settle to obtain a silica gel chromatography column;

[0016] 2) Weigh 20 g of Gentiana crude extract and dissolve it with a small amount of ethanol, add 60 g of 200-mesh silica gel and mix well, evaporate the solvent, dry in the air, grind through a 200-mesh sieve, and add to the silica gel chromatography column in step 1);

[0017] 3) Use a mixed solvent of chloroform and methanol with a volume ratio of 9:1 as the eluent for elution, and pure gentiopicroside as a control, follow-up detection by thin-layer chromatography, and collect and wash when a single spot of gentiopicroside appears. Drain until other spots reappear in the eluate and ...

Embodiment 2

[0021] The method for separating and purifying gentiopicroside of the present embodiment adopts the following steps:

[0022] 1) Weigh 600 g of 250-mesh column chromatography silica gel, add a mixed solvent of chloroform and methanol with a volume ratio of 9:1, stir until there are no bubbles, pour it into a glass chromatography column, and settle to obtain a silica gel chromatography column;

[0023] 2) Weigh 20 g of Gentiana crude extract and dissolve it with a small amount of ethanol, add 60 g of 250-mesh silica gel and mix well, evaporate the solvent, dry in the air, grind through a 200-mesh sieve, and add to the silica gel chromatography column in step 1);

[0024] 3) Use a mixed solvent of chloroform and methanol with a volume ratio of 9:1 as the eluent for elution, and pure gentiopicroside as a control, follow-up detection by thin-layer chromatography, and collect and wash when a single spot of gentiopicroside appears. Drain until other spots reappear in the eluate and ...

Embodiment 3

[0028] The method for separating and purifying gentiopicroside of the present embodiment adopts the following steps:

[0029] 1) Weigh 600 g of 280-mesh column chromatography silica gel, add a mixed solvent of chloroform and methanol with a volume ratio of 9:1, stir until there are no bubbles, pour it into a glass chromatography column, and settle to obtain a silica gel chromatography column;

[0030] 2) Weigh 20 g of Gentiana crude extract and dissolve it with a small amount of ethanol, add 60 g of 280-mesh silica gel and mix well, evaporate the solvent, dry in the air, grind through a 200-mesh sieve, and add to the silica gel chromatography column in step 1);

[0031] 3) Use a mixed solvent of chloroform and methanol with a volume ratio of 9:1 as the eluent for elution, and pure gentiopicroside as a control, follow-up detection by thin-layer chromatography, and collect and wash when a single spot of gentiopicroside appears. Drain until other spots reappear in the eluate and ...

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Abstract

The invention discloses a method for separating and purifying gentiamarin. A slica-gel column chromatography is adopted, wherein the particle size of column chromatography silica gel is 200 to 300 meshes, the using amount of the column chromatography silica gel is 30 times that of the weight of gentiamarin crude extract, eluent is mixed solvent of chloroform and ethanol in a volume ratio of 9:1, tracking and detection are performed by thin-layer chromatography by using a gentiamarin pure product as a contrast, the eluent is collected selectively, and the solvent is volatilized completely so as to obtain the gentiamarin pure product. By the slica-gel column chromatography, the particle size of the column chromatography silica gel, and the using amount of the eluent, the silica gel and the column chromatography silica gel are optimized, and gentiamarin can be separately eluted from a slica-gel chromatographic column in quantity according to the structural characteristics of gentiamarin, so that the extraction amount of gentiamarin is increased, and the purity of the finally obtained gentiamarin can reach 98.3 to 99.1 percent.

Description

technical field [0001] The invention relates to a method for separating and purifying gentiopicroside, in particular to a method for separating high-purity gentiopicroside from gentiana crude extract with 30% gentiopicroside. Background technique [0002] Gentiopicroside structural formula [0003] Gentiopicroside belongs to the split ring iridoid glycosides, which has anti-inflammatory, analgesic, hepatoprotective and choleretic effects, and is used for the treatment of rheumatic joint pain, tuberculosis hot flashes, infantile malnutrition fever, icteric hepatitis, urinary Unfavorable symptoms, gentiopicroside has been used by the Chinese Pharmacopoeia 2005 as a quantitative chemical indicator for the determination of gentian HPLC method, and it is also a symbolic component of the fingerprints of gentian and its products. Therefore, high-purity gentiopicroside is widely used and in great demand. [0004] Currently reported methods for the separation and purification of ...

Claims

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Application Information

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IPC IPC(8): C07H17/04C07H1/08
Inventor 段文录王洪斌陈彬刘普尹卫平
Owner HENAN UNIV OF SCI & TECH
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