Extraction separation method of ginkgolides

A technology of ginkgolide and separation method, which is applied in the directions of medical raw materials, pharmaceutical formulations, organic active ingredients and the like derived from Ginkgo biloba, can solve the problem that there is no process report, no pharmacology, toxicology and clinical test data, and the composition ratio of ginkgolide. question of uncertainty

Active Publication Date: 2012-09-12
CHENGDU BAIYU PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

None of these methods can effectively separate high-content ginkgolides, and the composition ratio of ginkgolides is uncertain. Therefore, the efficacy varies in clinical use. Due to its low content, there are also certain safety risks. There is no complete pharmacology, toxicology and clinical trial data. Therefore, the above methods are in the experimental stage and have not been implemented in the drug production process. Although there are related patents for ginkgolide injection in China, their composition is different from the present invention. According to ICH Searches on many official websites of member states have found that no other ginkgolide injection products have been listed so far
Currently, HPLC-UV, HPLC-MS and HPLC-ELSD methods are mostly used for the determination of ginkgolides. These methods can only measure the content of ginkgolides. Control does not truly reflect the quality characteristics of the drug, and does not form a complete drug quality control system. Although th

Method used

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  • Extraction separation method of ginkgolides
  • Extraction separation method of ginkgolides
  • Extraction separation method of ginkgolides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0101] Ginkgo biloba coarse powder 50kg, add 65% ethanol and heat and reflux extract 3 times (10, 8, 6 times the amount), each time for 1.5 hours, combine the extracts, filter, concentrate under reduced pressure, add 0.05% methionine and stir to dissolve, use citrate Adjust the pH value of the citric acid solution to 4-5, continue to concentrate, place at low temperature, and filter. First extract with an equal amount of n-hexane, then extract with an equal amount of ethyl acetate, and finally extract with a water-saturated sec-butanol-ethyl acetate mixed solvent, pass through a polyamide (30-60 mesh) resin column, first elute with water, and then use 30% ethanol was used for elution, and then 70% ethanol was used for elution, and the eluents were combined and concentrated under reduced pressure. Add 2 to 3 times the amount of boiling water, stir to dissolve, stand still, let cool, extract with ethyl acetate, concentrate under reduced pressure, add ethanol to heat and stir to ...

Embodiment 2

[0103] Ginkgo biloba coarse powder 200kg, add 6 times the amount of 80% ethanol and heat and reflux extract 3 times, each time for 1.5 hours, combine the extracts, filter, and recover the ethanol from the filtrate under reduced pressure until it has no alcohol smell, add 0.05% methionine and stir to dissolve, use cedar Adjust the pH value of the citric acid solution to 4-5, continue to concentrate, place at low temperature, and filter. First extract with n-hexane, then extract with ethyl acetate, and finally extract with water-saturated sec-butanol-ethyl acetate mixed solvent, pass through a polyamide (30-60 mesh) resin column, first elute with 30% ethanol, and then use 70 % ethanol was used for elution, and the eluents were combined and concentrated under reduced pressure. Add in boiling water, stir to dissolve, let stand to cool, extract with ethyl acetate, concentrate under reduced pressure, add ethanol to heat and stir to dissolve, filter, let cool, precipitate crystals, f...

Embodiment 3

[0105] Ginkgo biloba coarse powder 200kg, add 8 times the amount of 75% ethanol, heat and reflux extraction 3 times, each time for 1.5 hours, combine the extracts, filter, and recover the ethanol from the filtrate under reduced pressure until it has no alcohol smell, add 0.05% methionine and stir to dissolve, use citrate Adjust the pH value of the citric acid solution to 4-5, continue to concentrate, place at low temperature, and filter. First extract with n-hexane, then extract with ethyl acetate, and finally extract with water-saturated sec-butanol-ethyl acetate mixed solvent, pass through a polyamide (30-60 mesh) resin column, first elute with 30% ethanol, and then use 75 % ethanol was used for elution, and the eluents were combined and concentrated under reduced pressure. Add in boiling water, stir to dissolve, let stand to cool, extract with ethyl acetate, concentrate under reduced pressure, add ethanol to heat and stir to dissolve, filter, let cool, precipitate crystals,...

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Abstract

The invention relates to the field of phytoextraction, in particular to an extraction separation method of ginkgolides. The ginkgolides with fixed components can be obtained through the extraction separation method. The ginkgolides obtained through the steps of extraction, column chromatography, crystallization and crystal mixing in the method comprises bilobalide (C15H1808) of 25.0%-50.0%, ginkgolide A (C20H24O9) of 20.0%-45.0%, ginkgolide B (C20H24O10) of 10.0%-30.0%, ginkgolide C (C20H24O11) of 5.0%-15.0%. The total quantity of the bilobalide, the ginkgolide A, the ginkgolide B and the ginkgolide C amounts for over 95% of the ginkgolides.

Description

technical field [0001] The invention relates to the field of plant extraction, in particular to a method for extracting and separating ginkgolides. Background technique [0002] Since the 1960s, many countries have used modern separation techniques to study the chemical components of Ginkgo biloba. Through pharmacological experiments and clinical verification, it has been found that the various biological activities of Ginkgo biloba are related to the specific chemical components contained in them. Dr.Willar Schwabe of Germany registered a simple extract of Ginkgo biloba for the first time, and applied for a patent in 1972 (W Schwabe DE 176708 and DE 2117429), named EGb761, for the treatment of cardiovascular and cerebrovascular diseases and nervous system diseases. Significant curative effect, and no toxic side effects, ginkgolides (ginkgolids) have strong platelet activating factor (PAF) antagonistic effect. The countries where ginkgo preparations are listed as therapeuti...

Claims

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Application Information

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IPC IPC(8): C07D493/22C07D493/20
CPCA61K36/16A61K2236/00A61K2236/30A61P7/02A61P9/00A61P25/00A61P37/00C07D493/20C07D493/22A61K31/365
Inventor 孙毅朱永红童正兵王婕
Owner CHENGDU BAIYU PHARMA CO LTD
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