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Preparation of koumine by silica gel chromatography

A technique for colloid base and silica gel chromatography, which is applied in the field of separation and preparation of colloid base, can solve the problems of low yield, cumbersome preparation means and the like, and achieves the effect of improving yield

Inactive Publication Date: 2012-10-17
SHANGHAI UNIV OF T C M +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved in the present invention is to provide a method for preparing gesine from kelp extract, so as to solve the technical problems of cumbersome preparation means and extremely low yield in the prior art

Method used

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  • Preparation of koumine by silica gel chromatography
  • Preparation of koumine by silica gel chromatography
  • Preparation of koumine by silica gel chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Embodiment 1 The preparation of kelezine

[0021] 1 kg of the medicinal material Gelkins, after removal of impurities, crushed into coarse powder, reflux extraction with 5 L of 70% ethanol for 3 times, each time for 2 hours, combined extracts, recovered solvent to obtain about 1 L of extracts.

[0022] The extract was extracted three times with 2L of ethyl acetate, the ethyl acetate layers were combined, and the solvent was recovered under reduced pressure to obtain about 40 g of extract A.

[0023] Extraction A is separated by silica gel column chromatography (silica gel is 100-200 mesh or 200-300 mesh column chromatography silica gel, the weight ratio of extract sample to silica gel is 1:30, and the silica gel column specification is Φ100*1000mm), and with chloroform: The methanol volume ratio was 50:1 for elution, and the eluent was eluted on a thin-layer silica gel plate (GF 254 ) spotting, developed with chloroform:methanol volume ratio of 10:1, placed under the u...

Embodiment 2

[0025] Embodiment 2 The preparation of kelezine

[0026] 1kg of the medicinal material Gelkins, after removal of impurities, was crushed into a coarse powder, the volume concentration was 95% ethanol 5L reflux extraction 3 times, each time for 2 hours, the extracts were combined, and the solvent was recovered to obtain about 2L of the extract.

[0027] The extract was extracted three times with 1 L of ethyl acetate, the ethyl acetate layers were combined, and the solvent was recovered under reduced pressure to obtain about 40 g of extract A.

[0028] Extraction A is separated by silica gel column chromatography (silica gel is 100-200 mesh or 200-300 mesh column chromatography silica gel, the weight ratio of extract sample to silica gel is 1:50, and the silica gel column specification is Φ100*1000mm), and with chloroform: The methanol volume ratio was 25:1 for elution, and the eluent was eluted on a thin-layer silica gel plate (GF 254 ) spotting, developed with chloroform:meth...

Embodiment 3

[0030] Example 3 Preparation of kelesine

[0031] 1kg of the medicinal material Gelkins, after removal of impurities, was crushed into a coarse powder, and the volume concentration was 5L of 80% ethanol for reflux extraction for 3 times, each time for 2 hours, the extracts were combined, and the solvent was recovered to obtain about 1L of the extract.

[0032] The extract was extracted three times with 0.5L ethyl acetate, the ethyl acetate layers were combined, and the solvent was recovered under reduced pressure to obtain about 35 g of extract A.

[0033] Extraction A is separated by silica gel column chromatography (silica gel is 100-200 mesh or 200-300 mesh column chromatography silica gel, the weight ratio of extract sample to silica gel is 1:30, and the silica gel column specification is Φ100*1000mm), and with chloroform: The methanol volume ratio was 40:1 for elution, and the eluent was eluted on a thin-layer silica gel plate (GF 254 ) spotting, developed with chlorofor...

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Abstract

The invention discloses a method for preparing koumine from Gelsemium elegans Benth extract product, comprising steps of: (1) ethyl acetate extraction; and (2) silica gel chromatography purification. The invention relates to a simplified technology for preparing koumine. The technology can greatly raise yield of koumine and can be used in industrial preparation of koumine.

Description

technical field [0001] The invention relates to a preparation method of koumine, in particular to a method for separating and preparing koumine from an extract of koumine. Background technique [0002] Gelsemium elegans (Gelsemium elegans Benth.) is a plant belonging to the genus Gelsemium elegans, which can be divided into two types: Chinese elegans and North American elegans. my country is rich in Fujian, Zhejiang, Guangxi, Guangdong, Hunan and other places, also known as heartbroken grass. Its medicinal part is the whole plant. It has the effects of expelling wind and attacking poison, reducing swelling and relieving pain. [0003] Gelkinine compounds are a class of compounds present in Gelkins, which have been proved to have good activity in tumor and analgesic aspects. It is clinically used to inhibit the growth of tumor cells, treat neuralgia, and locally dilate pupils, etc., which can be considered as one of the material basis for the efficacy of Gelkins. [0004]...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22
Inventor 梁爽冯怡阮克锋
Owner SHANGHAI UNIV OF T C M
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