Method for preparing high-purity ginkgolides

A high-purity technology of ginkgolidene lactones, which is applied in the field of separation and purification of high-purity ginkgolidene lactones, can solve problems such as methanol residues and product dehydration difficulties, and achieve the effect of reducing the dehydration load

Inactive Publication Date: 2012-06-13
JIANGSU BESCON PHARMA
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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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take 1000g of ginkgo biloba crude extract with a purity higher than 6%, and extract it with ethyl propionate after drying. After vacuum-drying the extract, 88 g of solid powder was obtained, and then recrystallized with anhydrous ethyl acetate in an amount of 300 ml, crystallized twice; the above-mentioned crystallized product was subjected to supercritical CO 2 The solvent was extracted and dried, the pressure was set at 9 MPa, the temperature was 60°C, and the time was 60 minutes; 38.9 g of ginkgolides with a purity of 98.8% were obtained.

Embodiment 2

[0017] Take 1000g of ginkgo biloba crude extract with a purity higher than 6%, dry it and extract it with ethyl propionate, the amount of ethyl propionate is 6L for recrystallization, the extraction temperature is 75°C, the time is 2 hours, and the extraction is 3 times ; After vacuum drying of the extract, 92g of solid powder was obtained, and then recrystallized with anhydrous ethyl acetate, and the consumption was 450ml, crystallized 2 times; the above-mentioned crystalline product was subjected to supercritical CO 2 The solvent was extracted and dried, and the working pressure was set at 12MPa, the temperature was at 50°C, and the time was at 45min; 40.3g of ginkgolides with a purity greater than 99.1% were obtained.

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PUM

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Abstract

The invention relates to a method for separating and purifying high-purity ginkgo terpene lactones, and the high-purity ginkgo terpene lactones are prepared by adopting a combined process of solvent extraction, recrystallization, supercritical CO2 extraction removal and drying, wherein an extraction solvent is ethyl propionate; anhydrous ethyl acetate is used as a recrystallization solvent; and a supercritical CO2 extraction removal solvent is adopted for drying. The purity of a product can be above 99%. The separation and purification process is simple in method, low in cost and easy for industrial production and application.

Description

1. Technical field [0001] The invention relates to a method for obtaining active components of high-purity natural products, in particular to a new method for separating and purifying high-purity ginkgo terpene lactones from ginkgo biloba crude extract. 2. Background technology [0002] Ginkgo biloba extract (GBE) has been included in the Pharmacopoeia of the People's Republic of China (2005 edition). The medicinal GBE produced according to this standard has the purity of total ginkgo flavonoids ≥ 24%, and the purity of total ginkgo lactones ≥ 6%. [0003] 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 foo...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCY02P20/54
Inventor 张文成樊恩生刘鹏程
Owner JIANGSU BESCON PHARMA
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