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Method for preparing ginsenoside Rh1

A technology of ginsenoside and methanol, which is applied in the field of preparation of ginsenoside Rh1, can solve the problems of no further separation and purification of ginsenoside, no high-purity ginsenoside Rh1, and increased processing procedures, so as to save cost and energy, and facilitate industrial production , the effect of simplifying the separation procedure

Active Publication Date: 2012-05-02
YUXI WINHEY BIO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this application, not only the reaction temperature is higher, the alkali is introduced in the process of removing impurities, which increases the subsequent treatment procedures, but also the cost is high, and the total glycosides are prepared without further separation and purification of ginsenoside Rh1
So far, there is no report about the preparation of high-purity ginsenoside Rh1

Method used

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  • Method for preparing ginsenoside Rh1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] A. Acid hydrolysis: Dissolve the triol group ginsenosides with a purity greater than 80% in 8 times the amount of water, add glacial acetic acid to make the concentration of glacial acetic acid reach 15%, put the above mixed solution in a water bath, and hydrolyze at 50°C 7 hours.

[0018] B. Deacidification: the hydrolyzate is cooled to room temperature, and deacidified by DM130 macroporous adsorption resin column chromatography. Elute with water at a flow rate of 8 ml / min until the effluent is neutral, then elute with 85% ethanol until no purple spots are detected by thin-layer chromatography.

[0019] C. Enrichment: the hydrolyzate after deacidification is concentrated, dried, dissolved with 68% methanol, added 2 times the amount of silica gel to mix the sample, evaporated methanol, dry-packed, separated by silica gel column chromatography, and separated by chloroform:methanol : water=8:2:0.2 as the mobile phase, develop and elute. Thin-layer chromatography trackin...

Embodiment 2

[0022] A. Acid hydrolysis: Dissolve the triol group ginsenosides with a purity greater than 80% in 7 times the amount of water, add glacial acetic acid to make the concentration of glacial acetic acid reach 25%, put the above mixed solution in a water bath, and hydrolyze at 70°C 5 hours.

[0023] B, deacidification: the hydrolyzate is cooled to room temperature, deacidification with D101 macroporous adsorption resin column chromatography, water elution, flow rate 10ml / min, until the effluent is neutral, be 88% ethanol elution with concentration, until There was no purple spot detected by TLC.

[0024] C. Enrichment: the hydrolyzate after deacidification is concentrated, dried, dissolved with 70% methanol, added 2 times the amount of silica gel to mix the sample, evaporated methanol, dry-packed, separated by silica gel column chromatography, and separated by chloroform:methanol : water = 8: 2: 0.2 as the mobile phase, developing, elution, T thin layer chromatography tracking d...

Embodiment 3

[0027] A. Acid hydrolysis: Dissolve ginsenosides of the triol group with a purity greater than 80% in 9 times the amount of water, add glacial acetic acid to make the concentration of glacial acetic acid reach 18%, put the above mixed solution in a water bath, and hydrolyze at 58°C 6 hours.

[0028] B. Deacidification: Cool the hydrolyzate to room temperature, deacidify with DM130 macroporous resin column chromatography, elute with water at a flow rate of 11ml / min, until the effluent is neutral, rinse with 90% ethanol to a thin layer Chromatographic detection without purple spots.

[0029] C. Enrichment: the hydrolyzate after deacidification is concentrated, dried, dissolved with 71% methanol, added 2 times the amount of silica gel to mix the sample, evaporated methanol, dry-packed, separated by silica gel column chromatography, and separated by chloroform:methanol : Water = 8: 2: 0.2 as the mobile phase, developed, eluted, tracked and detected by thin-layer chromatography, a...

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Abstract

The invention discloses a method for preparing ginsenoside Rh1. Although the acid-hydrolysis method is applied to the preparation of total saponins and preparation thereof from ginsenoside, the complex procedure is needed for deacidification after acid-hydrolysis and no reports indicate that the special method for preparing high-purity Rh1 exists. The invention provides a method for preparing ginsenoside Rh1, which is characterized by comprising the steps of adding glacial acetic acid in protopanaxtriolsaponins for hydrolysis, obtaining Icariside part enriched with ginsenoside Rh1 by chromatography deacidification of macroporous resin column, carrying out purification by reversed-phase medium-pressure column chromatography, and finally obtaining the ginsenoside Rh1 with the purity of morethan 90%. The method adopts the macroporous resin column for chromatography deacidification, ensures high metastasis rate of the total saponins, has moderate hydrolysis condition and short reaction period, effectively saves cost and energy resource, is easy for industrial production, thus ensuring the high yield of Rh1 and improving purity.

Description

technical field [0001] The invention belongs to the technical field of natural medicine preparation, and in particular relates to a preparation method of ginsenoside Rh1. Background technique [0002] Discovering new drugs or physiologically active lead compounds from natural products is an important direction of drug research and development today. The dammarane-type tetracyclic triterpene glycosides in medicinal plants of the genus Panax genus Araliaceae have various physiological functions and have always been one of the hot spots of attention. Ginsenosides can be divided into protopanaxadiol type and protopanaxatriol type according to the chemical structure of their aglycones. The diol type is represented by Rb1, and the triol type is represented by Rg1. Ginsenoside Rh1 belongs to protopanaxatriol-type saponins, which can initiate and enhance immune response, promote liver cell proliferation, promote DNA synthesis, kill tumor cells, inhibit tumor cell proliferation, ind...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J17/00
Inventor 杨崇仁丁艳芬李立妍
Owner YUXI WINHEY BIO TECH
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