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Method for preparing bilobalide, bilobalide A, bilobalide B and bilobalide C

A technology of ginkgolide and bilobalide, applied in the preparation of ginkgolide B and ginkgolide C, bilobalide, ginkgolide A field, can solve the problem of the purity and yield of ginkgolide A and ginkgolide B Low yield and other problems, to achieve the effect of large amount of preparation and simple preparation process

Active Publication Date: 2016-07-27
JIANGSU KANION PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the refining method of this ginkgolide A and ginkgolide B provided by the prior art has simple process and less loss, it can simultaneously separate and purify ginkgolide A and ginkgolide B, but this method prepares ginkgolide A and the purity and yield of ginkgolide B are lower

Method used

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  • Method for preparing bilobalide, bilobalide A, bilobalide B and bilobalide C
  • Method for preparing bilobalide, bilobalide A, bilobalide B and bilobalide C
  • Method for preparing bilobalide, bilobalide A, bilobalide B and bilobalide C

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preparation example Construction

[0035] The invention provides a preparation method of bilobalide, ginkgolide A, ginkgolide B and ginkgolide C, comprising:

[0036] Ginkgo biloba is refluxed and extracted with an alcohol compound, filtered, concentrated, dispersed, and filtered again to obtain a filtrate;

[0037] After the filtrate is extracted, it is concentrated and dried successively to obtain the crude product of total ginkgo lactones;

[0038] The crude ginkgo lactones are mixed with silica gel in a solvent and pulverized to obtain sample silica gel;

[0039] The sample silica gel is subjected to gradient elution in a vacuum liquid chromatography separation device, and the eluent in the gradient elution process includes a weak polar solvent A and a strong polar solvent B, and the weak polar solvent A and The elution ratio of strong polar solvent B is (8.2~7.8): (1.8~2.2), and bilobalide is obtained; the elution ratio of described weak polar solvent A and strong polar solvent B is (7.2~6.8) : (3.2~2.8)...

Embodiment 1

[0087]Get 20Kg Ginkgo biloba medical material and adopt mass concentration to be that 75% ethanol solution reflux extracts twice (2h / time), the quality of described ethanol solution is 10 times that Ginkgo biloba medical material is prepared; The extract that obtains is filtered, merge twice filtrate Concentrate the combined filtrate under reduced pressure until there is no alcohol smell; add the obtained concentrated solution to water for dispersion, and the amount of the water is the same as that of the concentrated solution; filter the obtained dispersion to remove insolubles, and obtain clarification The filtrate; The clarified filtrate obtained is added to an equal volume of ethyl acetate to extract 3 times, and the product after the merging and extraction is concentrated and dried to obtain 245 g of ginkgo lactone crude product.

[0088] Dissolve 200 g of crude ginkgo lactones in methanol, add 90-mesh silica gel with the same quality as the crude total ginkgo lactones to ...

Embodiment 2

[0098] Get 20Kg Ginkgo biloba medical material and adopt mass concentration and be that 75% methanol solution reflux extracts twice (2h / time), the quality of described ethanol solution is 10 times that Ginkgo biloba medical material is prepared; The extract that obtains is filtered, merge twice filtrate Concentrate the combined filtrate under reduced pressure until there is no alcohol smell; add the obtained concentrated solution to water for dispersion, and the amount of the water is the same as that of the concentrated solution; filter the obtained dispersion to remove insolubles, and obtain clarification The filtrate; The clarified filtrate obtained is added to an equal volume of ethyl acetate to extract 3 times, and the product after the merging and extraction is concentrated and dried to obtain 262 g of ginkgo lactone crude product.

[0099] Dissolve 200 g of crude ginkgo lactones in ethanol, add 80-mesh silica gel with the same quality as the crude total ginkgo lactones t...

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Abstract

The invention provides a method for preparing bilobalide, bilobalide A, bilobalide B and bilobalide C.The method comprises the steps that ginkgo leaves are treated, and crude total terpene lactones are obtained; the crude total terpene lactones are mixed with silica gel, and a silica gel sample is obtained; the silica gel sample is subjected to gradient eluting in a vacuum liquid chromatogram separating unit, the eluting ratio of a weak polar solvent A to a strong polar solvent B in the gradient eluting process is (8.2-7.8):(1.8-2.2), and bilobalide is obtained; when the eluting ratio is (7.2-6.8):(3.2-2.8), bilobalide C is obtained; when the eluting ratio is (6.2-5.8):(4.2-3.8), bilobalide A is obtained; when the eluting ratio is 1:(0.5-1.5), bilobalide B is obtained.The yield and purity of bilobalide, bilobalide A, bilobalide B and bilobalide C prepared through the method are high.

Description

technical field [0001] The invention relates to the technical field of ginkgo, in particular to a preparation method of bilobalide, ginkgolide A, ginkgolide B and ginkgolide C. Background technique [0002] Ginkgolide (English name: ginkgolide) compounds belong to terpenoids, composed of sesquiterpene lactones and diterpene lactones, and are an important class of active ingredients in Ginkgo biloba leaves. Bilobalide (BB) is a sesquiterpene lactone, which is the only sesquiterpene lactone compound found in Ginkgo biloba. Ginkgolide A (ginkgolideA; GA), ginkgolide B (ginkgolideB; GB), ginkgolide C (ginkgolideC; GC), ginkgolide M (ginkgolideM; GM), ginkgolide J (ginkgolideJ; GJ) are Diterpenoids differ in the number of hydroxyl groups they contain and the positions at which the hydroxyl groups are attached. Ginkgolide molecule has a unique twelve-carbon skeleton structure, embedded with a tert-butyl group and six five-membered rings, including a spirononane, a tetrahydrofura...

Claims

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Application Information

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IPC IPC(8): C07D493/22C07D493/20
CPCC07D493/20C07D493/22
Inventor 萧伟倪付勇刘露赵祎武宋亚玲温建辉谢雪黄文哲王振中
Owner JIANGSU KANION PHARMA CO LTD
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