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Method for preparing ginkgolide compound

A technology of ginkgolide and compound, applied in the field of medicine, can solve the problems of high production requirements, difficult industrialized production and high cost

Inactive Publication Date: 2010-06-23
广州艾格生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has improved compared with the previous technology, the overall extraction efficiency has increased by 10%, but industrialization is still relatively difficult, and the cost is still high, so it is difficult to industrialize
The patent No. CN101054384A discloses a purification method of lactone B, which requires two column chromatography in the process, and the transfer rate of ginkgolide B component is less than 2%, and the cost is relatively high
The patent No. CN101302222A discloses that the transfer rate of ginkgolide B component reaches 15%. Although it has been greatly improved, the production cost according to this process is still too high
On the whole, the extraction rate or transfer rate of ginkgolide compounds obtained at present is below 15%, the production requirements are relatively high, the production cost is relatively high, and industrial production is difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 10 kg of ginkgo leaves, add water to extract for 30 minutes, filter to obtain 300 L of extract, extract with 3000 L of petroleum ether, concentrate the extract to an appropriate amount, add an appropriate amount of 200-300 mesh silica gel, mix and dry, put on a silica gel column, and use petroleum ether Ether: ethyl acetate is the ratio preparation mobile phase of 1: 1 and carries out elution, collects and contains ginkgolide A 50L effluent, concentrates dry to obtain 11g dry cream, adds 110ml 95% ethanol crystallization, obtains 3.45g ginkgolide A, Among them, the content of ginkgolide A is 92.9%.

Embodiment 2

[0021] Weigh 10 kg of ginkgo leaves, add citric acid to adjust the pH of the water to 4.5, extract for 60 minutes, filter to obtain 500 L of extract, extract with 2000 L of n-butanol, concentrate the extract to an appropriate amount, add an appropriate amount of 300-400 mesh silica gel, and mix well Oven dry, go up silica gel column, with n-butanol: acetone is the ratio preparation mobile phase of 6: 4 and carry out elution, collect and contain ginkgolide B 40L effluent, concentrate and dry to obtain 9g dry paste, add 150ml95% ethanol crystallization, obtain 2.28g of ginkgolide B, wherein the content of ginkgolide B is 102.1%.

Embodiment 3

[0023] Weigh 10 kg of ginkgo leaves, add sodium acetate to adjust the pH of the water to 8.5, extract for 40 minutes, filter to obtain 200 L of extract, extract with 2500 L of n-hexane, concentrate the extract to an appropriate amount, add an appropriate amount of 200-300 mesh silica gel, mix and dry Dry, put on a silica gel column, elute with ethyl acetate, collect 60L effluent containing ginkgolide C, concentrate and dry to obtain 14g dry cream, add 150ml95% ethanol to crystallize, obtain 2.92g ginkgolide C, wherein, ginkgolide The C content is 95.9%.

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PUM

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Abstract

The invention relates to a method for preparing ginkgolide compound, belonging to the medicine field. The invention is characterized in that ginkgolide compound raw materials are prepared through the following method that: ginkgo leaves or ginkgo leaf extracts are taken and are extracted in aqueous solution, the obtained extract liquid is filtered and is extracted by using organic solvent, the obtained extract liquid is concentrated and is mixed with 200-mesh to 1,000-mesh silica gel, the obtained mixture is dried, eluent rich in ginkgolide compound is collected by adopting silica column chromatography, the collected eluent is crystallized to respectively obtain ginkgolide A, ginkgolide B, ginkgolide C, ginkgolide J, ginkgolide M and ginkgolide K raw materials, and the contents are respectively 90 percent to 110 percent. The invention has the advantages that the purity of the ginkgolide compound prepared through the method is high; and the preparation process is simple, the transfer rate is high, the cost is low and the industrial scale production can be realized.

Description

technical field [0001] The invention belongs to the field of medicine, and in particular relates to a preparation method of ginkgolide compounds. technical background [0002] Ginkgolides are the main active ingredients in Ginkgo biloba and Ginkgo biloba extracts (EGB761, CP2000, CP2005), including ginkgolides and bilobalides, of which ginkgolides mainly include ginkgolides A, B, C, J, M and K monomers, according to literature reports, ginkgolide is a specific platelet activating factor (PAF) receptor blocker, which can eliminate the platelet aggregation caused by PAF in a dose-dependent manner, thereby preventing the formation of thrombus. The latest pharmacological studies have shown that ginkgolides have anti-allergic, anti-inflammatory, anti-shock effects, and also have protective effects on ischemic injury and organ transplant rejection. Bilobalide has a unique curative effect on the treatment of nervous system diseases. In order to improve the therapeutic effect and r...

Claims

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Application Information

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IPC IPC(8): C07D493/22A61K36/16
Inventor 李玉梅
Owner 广州艾格生物科技有限公司
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