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Chinese magnoliavine fruit monomer composition separation preparation method

A technology of Schisandra chinensis and Schisandra chinensis ester B, which is applied in the field of countercurrent chromatography preparation and separation, can solve the problems of difficulty in obtaining high-purity samples, cumbersome operations, and low separation efficiency, and achieve technological innovation and improvement, solvent saving, and high product purity. Effect

Inactive Publication Date: 2012-09-26
华美恒盛(北京)科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the separation of biphenyl cyclooctene lignans mostly uses column chromatography, but the operation is very cumbersome, and the separation efficiency is not high, and it is difficult to obtain high-purity samples

Method used

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  • Chinese magnoliavine fruit monomer composition separation preparation method
  • Chinese magnoliavine fruit monomer composition separation preparation method
  • Chinese magnoliavine fruit monomer composition separation preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1.3Kg of the schisandra medicinal material was pulverized, extracted with 80% ethanol under reflux, and the extract was concentrated under reduced pressure to obtain a concentrated solution. The concentrated solution was extracted with petroleum ether to obtain 89 g of extract. The petroleum ether extract was subjected to silica gel column chromatography, petroleum ether-ethyl acetate=3:1 (V / V) isocratic elution, monitored by HPLC, the same parts were combined, and the solvent was recovered to obtain 9.2g of crude extract A and 74.6g crude extract B.

[0022] The crude extract A is separated by high-speed countercurrent chromatography, and the solvent system n-hexane-ethyl acetate-methanol-water is selected. First, the above-mentioned solvent system is configured in a separatory funnel with a volume ratio of 18:1:20:1.2, and shaken After uniformity, let it stand for stratification. After equilibrating for 12 hours, separate the upper and lower phases. Take the upper ph...

Embodiment 2

[0029] Pulverize 1.3 kg of Schisandra medicinal material, extract with 95% ethanol under reflux, and concentrate the extract under reduced pressure to obtain a concentrated solution. The concentrated solution was extracted with petroleum ether to obtain 96g of extract. The petroleum ether extract was subjected to silica gel column chromatography, petroleum ether-ethyl acetate=5:1 (V / V) isocratic elution, HPLC monitoring, the same parts were combined, and the solvent was recovered to obtain 8.0 g of crude extract A and 85.1 g crude extract B.

[0030] The crude extract A is separated by high-speed countercurrent chromatography, and the solvent system n-hexane-ethyl acetate-methanol-water is selected. First, the above-mentioned solvent system is configured in a separatory funnel at a volume ratio of 20:1:20:1, and shaken After uniformity, let it stand for stratification. After equilibrating for 12 hours, separate the upper and lower phases. Take the upper phase as the stationar...

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Abstract

The invention relates to a Chinese magnoliavine fruit monomer composition separation preparation method; ethanol extracts from Chinese magnoliavine fruit are extracted by petroleum ether, chromatography is carried out to the petroleum ether extracts by a silicagel column, and then the petroleum ether is eluted by petroleum ether-ethylacetate, and HPLC is used for monitoring, and then crude extract A and crude extract B are fraction-collected, and eluted; the volume ratio of eluant petroleum ether and ethylacetate is 3-5:1, the crude extract A and crude extract B are respectively applied to a high-speed counter-current chromatography for separation, so as to obtain SCHisanhenol, deoxyschizandrin, schizandrin B, schisandrin C, schizandrol A, schizandrol B and schisantherrin B monomers, and the purity is higher than 98 percent.

Description

Technical field: [0001] The invention relates to a countercurrent chromatography preparation and separation method, in particular to a method for separating and preparing schisandra lignan monomer components from 70-95% ethanol crude extract of Schisandra chinensis by applying high-speed countercurrent chromatography. Background technique: [0002] Schisandra chinensis (Turcz.) Baill. is the dry mature fruit of Schisandra chinensis (Turcz.) Baill., which is listed as the top grade in herbal medicine. Modern pharmacological studies have shown that schisandra can increase central nervous excitement, enhance human spirit, physical strength, cardiovascular system tension and cardiac contractility, and reduce serum alanine enzyme activity in patients with viral hepatitis. The main chemical components are lignans, triterpenes, sesquiterpene organic acids, volatile oils and polysaccharides. Biphenylcyclooctene lignans are the main active components in Schisandra chinensis, which h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D317/70C07C43/253C07C43/235C07C37/72
Inventor 张天佑孙庆武张文晋王晓
Owner 华美恒盛(北京)科技有限公司
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