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Ginkgolide B raw material and preparation method thereof

A technology of ginkgolides and raw materials, applied in the field of traditional Chinese medicine extracts, can solve the problems of ginkgolide B monomer purity is not high enough, can not be used as injection raw materials, and is not suitable for industrial production, so as to improve the utilization of raw materials and large application The effect of controllable value and quality

Inactive Publication Date: 2019-12-31
SHANGHAI SINE PROMOD PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Because the purity of the ginkgolide B monomer extracted in the prior art is not high enough, it can only be used as a raw material for oral preparations and cannot be used as an injection bulk drug, or although it can reach a higher purity, the method used is not suitable for Industrial production

Method used

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  • Ginkgolide B raw material and preparation method thereof
  • Ginkgolide B raw material and preparation method thereof
  • Ginkgolide B raw material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] Take 500kg of dried Ginkgo biloba leaves, crush them, and extract them three times under reflux with 80% ethanol. The amount of solvent used is 4000L, 2500L and 2500L in sequence, and each extraction is 2h. Add 1000L of purified water, let it stand, filter, put the filtrate on a macroporous adsorption resin column (D101), wash the column with purified water (1500L) to remove impurities, and elute with 70% ethanol (2000L) until the color of the eluent becomes light. Concentrate under reduced pressure (-0.09Mpa) at 60°C, and dry at 60°C for 4 hours to obtain Ginkgo biloba extract (10.5kg). The content of total ginkgo lactones detected by HPLC-ELSD (High Performance Liquid Phase-Evaporative Light Scattering Detector) is 8.1 %.

Embodiment 2

[0047] Take 500kg of dried ginkgo leaves, crush them, and extract them three times under reflux with 70% ethanol. Purified water 1000L, stand still, filter, the macroporous adsorption resin column (D101) is put on the filtrate, purified water (1500L) washes the column to remove impurities, 65% ethanol (2200L) is eluted until the color of the eluate becomes light, and the eluate is in Concentrate under reduced pressure at 60° C., and dry at 60° C. for 4 hours to obtain a ginkgo leaf extract (10.6 kg). The content of total ginkgo lactones detected by HPLC-ELSD is 7.5%.

Embodiment 3

[0049] Get 500kg of dry ginkgo leaves, pulverize, 80% ethanol reflux extraction once, the solvent consumption is 4000L, then 70% ethanol reflux extraction once, solvent consumption is 3000L, extract 2h each time, combine the extracts, reduce pressure at 60 ℃ (-0.09Mpa ) concentrated to no ethanol smell, add 1000L of purified water, let stand, filter, the filtrate is put on a macroporous adsorption resin column (D101), washed with purified water (1500L), and then eluted with 25% ethanol for 1500L to remove impurities, 65% ethanol (2200L) was eluted until the color of the eluate became lighter, and the eluate was concentrated under reduced pressure at 60°C, and dried at 60°C for 4 hours to obtain Ginkgo biloba extract (11.3kg). The content of total ginkgo lactones detected by HPLC-ELSD was 8.7 %.

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Abstract

The invention relates to a ginkgolide B raw material and a preparation method thereof. The ginkgolide B raw material is extracted from ginkgo leaves, the content of a ginkgolide B compound in the ginkgolide B raw material is greater than 99%, and the ginkgolide B raw material contains trace ginkgolide component ginkgolide HK, ginkgolide K and ginkgolide A, and the content is less than 0.4%. The invention also relates to a preparation method of the ginkgolide B raw material, and the method includes the steps of: extracting ginkgo leaves to obtain a ginkgo leaf extract, dissolving the extract with water, performing extraction with an organic solvent to obtain an extract, then adding hydrous ethanol / methanol for repeated crystallization to obtain a refined product I; recrystallizing the coarse crystallization mother liquor part repeatedly to obtain a refined product II, and combining and mixing the refined product I and the refined product II uniformly to obtain the product. The inventionprovides the basis for deep research of the ginkgolide B compound, the adopted reagents are safe and environment-friendly and recyclable, and the yield is improved, therefore the ginkgolide B raw material has great market application prospect.

Description

technical field [0001] The invention relates to extracts of traditional Chinese medicines, in particular to monomers of extracts of traditional Chinese medicines, in particular to a ginkgolide B raw material and a preparation method thereof. Background technique [0002] Ginkgolide B, English name Ginkgolide B; molecular formula: C20H24O10; molecular weight: 424.40. [0003] Ginkgolide B is a highly active platelet activating factor (PAF) antagonist, which can competitively bind to the PAF receptor and inhibit the action of PAF; therefore, any disease related to PAF, such as: thrombosis, cerebral Ginkgolide B has a certain curative effect on tissue damage, organ transplant rejection, acute inflammation, cardiac allergy, cellular endotoxin and shock caused by IgG. [0004] CN101182325A relates to a kind of intravenous administration of ginkgolide B and its extraction method, wherein the content of ginkgolide B is more than 97%, ginkgolic acid is less than or equal to 2PPM, a...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 肖志勇李丁李玉杰陈芸王宁胡林森
Owner SHANGHAI SINE PROMOD PHARMA
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