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Preparation method of nontoxic high-purity ginkgo total lactones and monomers thereof

A technology of total ginkgolides and ginkgolides, which is applied in the field of preparation of high-purity total ginkgolides and its monomers, can solve problems such as methanol residues and difficult product dehydration, and achieve the effect of promoting development

Active Publication Date: 2015-11-18
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses ethanol water or methanol crystallization, the product is difficult to dehydrate and may have methanol residue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Dissolving: Weigh 100g of commercially available ginkgolide crude extract with a purity of 70.6% (GA purity 33.4%, GB purity 29.7%, GC purity 7.5%) raw materials, according to the liquid-solid ratio of 20:1 (V / W) , that is, dissolve in 2L of warm water (40°C);

[0035] (2) Extraction: extract with propyl formate as solvent, the volume ratio of above-mentioned solution and propyl formate extraction solvent is 1:1, extract 2 times;

[0036] (3) Precipitation: the extract is concentrated to about 1L, and petroleum ether is added for precipitation, the volume of petroleum ether is 30% of the volume of the extraction concentrate, and the precipitate is total ginkgo lactones with a purity of 98.3%.

[0037] (4) Compatible packing column chromatography: using neutral alumina and normal phase silica gel composite packing, the mass ratio of alumina to silica gel is 1:3, and the eluent is a mixture of propyl formate and petroleum ether (propyl formate: petroleum Ether=2:1, V...

Embodiment 2

[0040] (1) Dissolving: Weigh 100g of commercially available ginkgolide crude extract with a purity of 70.6% (GA purity 33.4%, GB purity 29.7%, GC purity 7.5%) raw materials, according to the liquid-solid ratio of 22:1 (V / W) , that is, dissolve in 2.2L of warm water (40°C);

[0041] (2) Extraction: extract with propyl formate as solvent, the volume ratio of above-mentioned solution and propyl formate extraction solvent is 1:1, extract 2 times;

[0042] (3) Precipitation: the extract is concentrated to about 1.1L, and petroleum ether is added for precipitation, the volume of petroleum ether is 30% of the volume of the extraction concentrate, and the precipitate is total ginkgo lactones with a purity of 98.8%;

[0043] (4) Compatible packing column chromatography: using neutral alumina and normal phase silica gel composite packing, the mass ratio of alumina to silica gel is 1:3, and the eluent is a mixture of propyl formate and petroleum ether (propyl formate: petroleum Ether=1:...

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Abstract

The invention relates to a preparation method of nontoxic high-purity ginkgo total lactones and monomers thereof, which adopts a solvent extraction+precipitation+compound filled column chromatography+supercritical CO2 back extraction crystallization combined technique to prepare the high-purity ginkgo total lactones and monomers thereof. The extraction solvent is propyl formate, the precipitation solvent adopts petroleum ether, and the total lactone purity is up to 98%. The neutral aluminum oxide / normal-phase silica gel compound filled column chromatography is performed, and the supercritical CO2 back extraction crystallization is performed to obtain the ginkgo lactone monomers A, B and C with the purity of 97% or above; and no toxic ginkgolic acid is detected. The separation purification technique has the advantages of simple method and high product purity, and can be easily used in practical production.

Description

1. Technical field [0001] The invention relates to a method for extracting, separating and purifying active ingredients of natural products, in particular to a method for preparing high-purity total ginkgolides and monomers thereof from crude ginkgolide extracts. 2. Background technology [0002] Ginkgolides include ginkgolide A (hereinafter referred to as GA), ginkgolide B (hereinafter referred to as GB), ginkgolide C (hereinafter referred to as GC), ginkgolide J, ginkgolide M and bilobalide, etc. It is a unique ingredient of Ginkgo biloba. Ginkgolides, such as GA, GB, GC, etc., have a significant effect on the treatment of cardiovascular and cerebrovascular diseases. In order to develop new drugs or health foods with high efficiency and clear targets, it is necessary to separate ginkgolides with high purity. Ginkgolides are isolated from the crude extract of Ginkgolides. Ginkgolide crude extract is mainly extracted and separated from Ginkgo biloba leaves, but Ginkgo bil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22
CPCC07D493/22Y02P20/54
Inventor 张文成
Owner HEFEI UNIV OF TECH
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