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Preparation method of panaxadiol saponin and panaxadiol type saponin monomer

A technology of panaxadiol saponins and ginsenosides is applied in the preparation of steroids, the preparation of sugar derivatives, chemical instruments and methods, etc., and can solve the problems of strong dead adsorption, high cost of fillers, poor selectivity, etc., and achieves high separation, high The effect of large adsorption capacity and large loading capacity

Active Publication Date: 2017-09-22
云南特安呐制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the patent literature reports, the separation of ginseng diol saponins and their monomers from the root medicinal materials of Panax notoginseng, ginseng and American ginseng is mainly obtained by macroporous resin adsorption to obtain total saponins, and then the total saponins are separated and purified by silica gel column or gel column to obtain high purity. Panaxadiol saponins and panaxadiol saponin monomers Rb1, Rd; in these reports, most of the adsorption resins used are large-pore low-selectivity broad-spectrum styrene non-polar macroporous adsorption resins, which teach the desugaring function strong, but even if gradient elution is used to separate diol and triol saponins, the effect of separating diol and triol saponins is poor, and triol saponins are often entrained in diol saponins, which cannot achieve a good separation effect; the separation and preparation of ginseng diol monomers is mainly through normal Phase silica gel column chromatography or reverse phase C-18 silica gel column chromatography to obtain Rb1 and Rd monomers
The amount of organic solvent used in silica gel column chromatography is large, the dead adsorption is strong, and the yield and content of the obtained monomers are low. The use of C-18 silica gel column layer can largely solve the shortcomings of silica gel column chromatography. Tens of thousands of kilograms, the cost of filler is too high; in a word, the existing ginseng diol saponins and monomer extraction and separation have the disadvantages of poor selectivity, low separation purity, high cost, low yield, and not suitable for industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1: The preparation method of this Panaxadiol Saponin is as follows:

[0025] (1) After the American ginseng was crushed to 60 mesh, an ethanol solution with a concentration of 60% of crude drug mass 7 times the mass was added to the raw material and extracted by cold soaking at room temperature for 12 hours. % ethanol solution for extraction for 12 hours, and after filtration, add 3 times the mass percentage of the crude drug to the residue in an ethanol solution with a concentration of 60% for extraction for 12 hours; combine the three extracts and concentrate under reduced pressure at 60°C to recover the solvent, and dilute the concentrated solution to 5 times the crude drug with purified water Diatomaceous earth filter after measuring, collect filtrate;

[0026] (2) Pass the filtrate of step (1) through a macroporous adsorption resin (ZGCAD45) column with a pore size of 50-60 μm to adsorb ginseng triol saponins, collect the effluent from the upper column, ...

Embodiment 2

[0030] Embodiment 2: the preparation method of this Panaxadiol Saponin is as follows:

[0031](1) After ginseng is used as the raw material and crushed to 60 mesh, an ethanol solution with a concentration of 8 times the mass percentage of the crude drug is added to the raw material and extracted by cold soaking at room temperature for 12 hours. % ethanol solution for extraction for 12 hours, after filtration, add 4 times the mass percentage of the crude drug to the residue in an ethanol solution with a concentration of 70% for extraction for 12 hours; combine the 3 extracts and concentrate under reduced pressure at 60°C to recover the solvent, and dilute the concentrated solution to 4 times the crude drug with purified water Diatomaceous earth filter after measuring, collect filtrate;

[0032] (2) Pass the filtrate of step (1) through a 50-65 μm pore size macroporous adsorption resin (IIZ-803) column to adsorb ginseng triol saponins, collect the effluent from the upper column,...

Embodiment 3

[0036] Embodiment 3: the preparation method of ginseng diol type saponin monomer is as follows:

[0037] (1) After taking Panax notoginseng as the raw material and crushing it to 60 mesh, add an ethanol solution with a concentration of 75% of the mass percentage of the crude drug to 7.5 times the mass percentage of the raw material, cold soak and extract at room temperature for 12 hours, and add a concentration of 5.5 times the mass percentage of the crude drug mass to the filter residue after filtration Extract with 75% ethanol solution for 12 hours, add 3.5 times the mass percentage of crude drug to the filter residue to extract with 75% ethanol solution for 12 hours; combine 3 extracts and concentrate under reduced pressure to recover the solvent, and dilute the concentrated solution to 5 times the crude drug amount with purified water After diatomaceous earth filtration, collect filtrate;

[0038] (2) Pass the filtrate of step (1) through a macroporous adsorption resin (D4...

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PUM

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Abstract

The invention discloses a preparation method of a panaxadiol saponin and a panaxadiol type saponin monomer. The preparation method comprises the following steps: taking radix notoginseng, ginseng or American ginseng as raw materials, extracting and concentrating the raw materials through low alcohols and filtering through diatomite; then selectively absorbing panaxatriol saponin with macroporous resin with an aperture of 50-70 [mu]m, collecting effluent liquid and drying to obtain a panaxadiol saponin coarse product; dissolving the panaxadiol saponin coarse product through methanol, ethanol, methanol water or ethanol water, adding acetonitrile or ethyl acetate to precipitate, collecting a precipitate to dissolve, putting a panaxadiol saponin aqueous solution on a chromatographic resin column, firstly resolving triol impurities with an ethanol solution, and dissolving and resolving by adopting different concentrations of ethanol or methanol solutions to obtain the panaxadiol saponin or the panaxadiol type saponin monomer. The preparation method disclosed by the invention overcomes the defects of low yield, high production cost, low purity, long production period and the like in the prior art, obtains the high-purity panaxadiol saponin or the panaxadiol type saponin monomer and is simple and easy to operate, low in cost, suitable for industrial production, environment-friendly and free of pollution.

Description

technical field [0001] The invention relates to a preparation method of panaxadiol saponin and panaxadiol type saponin monomer. Background technique [0002] Panax notoginseng, ginseng, and American ginseng are precious Chinese medicinal materials in my country. The main components are ginsenosides. Body saponins can be divided into 20(S)-protopanaxadiol (panaxadiol Saponin, PDS) and 20(S)-protopanaxatriol Saponin, PTS) according to their structural characteristics. Protopanaxadiol saponins in Panax notoginseng, ginseng and American ginseng are mainly composed of ginsenosides Rb1 and Rd, protopanaxatriol saponins are mainly composed of ginsenosides Re and Rg1, and Panax notoginseng also includes notoginsenoside R1. [0003] The pharmacological effects of ginseng diol type saponins are as follows: 1. Improve cerebral blood circulation and protect brain tissue: expand blood vessels to reduce cerebral vascular resistance and increase internal carotid artery blood flow. Improve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H1/06C07H1/08C07H15/256C07J63/00C07J75/00
CPCC07H1/06C07H1/08C07H15/256C07J63/008C07J75/00
Inventor 张文生曾立品罗金明辛文锋蔡群虎刘石磊胡会泽杨雪王芬
Owner 云南特安呐制药股份有限公司
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