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Method for extracting ginkgolide B from gingkgo leaf or gingkgo leaf extract

A technology of ginkgolide and ginkgo leaf is applied in the field of preparation of ginkgolide B, which can solve the problems of low utilization rate of mobile phase and stationary phase, difficult industrialized production, low separation efficiency, etc., and achieves saving solvent consumption and strong pertinence , the effect of high product content

Active Publication Date: 2007-10-17
GUILIN NATURAL INGREDIENTS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, one way to produce ginkgolide B is to obtain products with higher content through multi-step separation. These separation processes include rough extraction processes such as leaching, filtration, extraction, and precipitation. There are still many impurities in the crude extract. Another method is to adopt resin column chromatography and aluminum oxide column chromatography. Resin column chromatography is a refining method that is often used in the medicine and food industry. This equipment is simple and the primary investment in equipment is low. The disadvantages are that the efficiency of separation is low, the utilization rate of mobile phase and stationary phase is low, the cost is high, the yield is low, and the contradiction between product content and yield is difficult to balance in column chromatography. To maintain the content, only sacrifice Yield, this low yield will inevitably lead to high cost; There is also a method that adopts simulated moving bed chromatography and recrystallization organic combination to obtain finished product through extraction, simulated moving bed purification, recrystallization, and the method yield is high (about 1.5%), high extraction rate (more than 60%), high content, but it is difficult to realize industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] One, take ginkgo extract (24% of total flavonoids, 6% of total lactones, 15-25 pomi degrees, produced by Guilin Rhine Biotechnology Co., Ltd.) as raw material;

[0031] 2. High-speed countercurrent extraction:

[0032] 1) Import the ginkgo extract or the concentrated extract into the extraction tower, and evenly add ethyl acetate from the bottom of the tower for convective solvent extraction. The amount of ethyl acetate is generally 1.5 times that of the liquid medicine, and the number of cycles is 4. Different towers body, collected separately;

[0033] 2) Recover the extracted ethyl acetate to obtain a thick paste, concentrate to 20°C, vacuum-dry at 65°C, and crush to 90-100 mesh to obtain ginkgolide product;

[0034] 3. Column chromatography and recrystallization:

[0035] 1) after dissolving the obtained ginkgolide with 75% ethanol, pass through a polyamide column of 80-120 mesh, and collect the effluent;

[0036] 2) Pass the effluent through the HP-20 macroporou...

Embodiment 2

[0039] 1. Ginkgo extract (powder: 24% of total flavonoids, 6% of total lactones, produced by Guilin Xingda Pharmaceutical Factory) is used as raw material, dissolved in 2 times the amount of purified water;

[0040] 2. High-speed countercurrent extraction:

[0041] 1) Import the ginkgo extract or the concentrated extract into the extraction tower, and evenly add ethyl acetate from the bottom of the tower for convective solvent extraction. The amount of ethyl acetate is generally twice that of the liquid medicine, and the number of cycles is 4. Different towers body, collected separately;

[0042] 2) recovering the extracted ethyl acetate to obtain a thick paste, concentrating to 22 degrees Celsius, vacuum drying at 70°C, and crushing to 90-100 mesh to obtain ginkgolide products;

[0043] 3. Column chromatography and recrystallization:

[0044] 1) Dissolving the obtained ginkgolide with 80% ethanol, passing through a polyamide column of 80-120 mesh, and collecting the effluen...

Embodiment 3

[0048]1. Take 100kg of fresh and dried ginkgo green leaves, dry them, control the temperature at 70°C, remove impurities, crush them, pass through a 60-mesh sieve, and extract them twice with 60% ethanol, the first time is 90 minutes, and the second time is 60 minutes. Combine the extracts, concentrate under reduced pressure, and recover ethanol; add 2 times the water to the concentrate, precipitate for 24 hours, centrifuge, take the supernatant and put it on an HP-20 adsorption column, wash it with water first, then elute with 80% ethanol, collect and wash Deliquified, concentrated.

[0049] 2. High-speed countercurrent extraction:

[0050] 1) Import the ginkgo extract or the concentrated extract into the extraction tower, and add ethyl acetate evenly from the bottom of the tower for convective solvent extraction. The amount of ethyl acetate is generally 2.5 times that of the liquid medicine, and the number of cycles is 5. Different towers body, collected separately;

[005...

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Abstract

The present invention discloses a preparation method for extracting bilobalide B from gingko leaf or its extract, which comprise: high speed countercurrent extraction, column chromatography for separation, recrystallization. The method can not only remove the harmful substance as alkylphenolic acids from gingko crude extract, but promote the yield of bilobalide B, promote the product content, and be suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of preparation of plant extracts, in particular to a preparation method for extracting ginkgolide B, an active ingredient of medicine, from ginkgo leaves or ginkgo leaf extracts. Background technique [0002] Ginkgo biloba (Ginkgo hiloba L.) is a plant of the genus Ginkgo in the Ginkgo family. With the deepening of research on Ginkgo biloba at home and abroad, it is found that Ginkgo biloba contains ginkgolides A, B, C, ginkgo flavonoids and other impurities, and the active ingredient Ginkgolide B in Ginkgo biloba is a kind of High-efficiency platelet-activating factor antagonists have unique pharmacological effects and therapeutic value, and can be used to treat stroke, shock, transplantation, hemodialysis, asthma and other diseases, and have aroused great interest in the pharmaceutical industry worldwide. In the production process of ginkgolide B, the most critical step is separation and purification. ...

Claims

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Application Information

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IPC IPC(8): C07D493/22A61K36/16
Inventor 孙步祥汤凌志李杰梁远胜杨文国蒋小三易永基
Owner GUILIN NATURAL INGREDIENTS CORP
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