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Process for preparing ginkgolide

A technology of ginkgolide and production process, which is applied in the field of ginkgolide production technology, can solve the problems of inconvenience, unsatisfactory quality, influence on product market supply and the like of ginkgolide, and achieves simple production equipment, high extraction yield and high technology The effect of easy operation of the route

Inactive Publication Date: 2004-09-22
SHANGHAI INST OF MATERIA MEDICA CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Ginkgolide A and Ginkgolide B This method will cause many problems in industrial production, and the unsatisfactory quality will affect the market supply of products. At present, the production technology of ginkgo leaf extract in China mainly adopts the technology of macroporous resin. Its highest The produced product quality of level is flavonoid glucoside ≥ 24%, total lactone ≥ 6% (wherein bilobalide ≥ 3%) ginkgolic acid < 1ppm, and the production method of ginkgolide adopts chromatographic method separation at present to large-scale production Ginkgolides bring a lot of inconvenience, and quality control has not yet found an ideal method

Method used

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  • Process for preparing ginkgolide
  • Process for preparing ginkgolide
  • Process for preparing ginkgolide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 500 grams of GBE (containing more than 6% of ginkgolides), heat-extract three times with water-saturated ethyl acetate, each time for 20 minutes, add 1750 ml of ethyl acetate each time, combine the ethyl acetate liquid, and use 500 ml of 1% NaHCO 3 Wash once with aqueous solution and once with 1% NaCl, taking into account NaHCO 3 and NaCl aqueous solution may take off the lactone, followed by sequential washing of NaHCO with ethyl acetate 3 and NaCl washing solution, combined all ethyl acetate solutions, concentrated under reduced pressure and dried in vacuo, the concentrate was dissolved in 90ml of 95% ethanol, and after dissolving, add 100ml of hot distilled water (60-70°C) while it was hot, and leave it overnight at room temperature, vacuum the next day Filter this solution, the crystallization that filters gets is 9: 10 solution washes with 95% ethanol: distilled water, vacuum-dried 12 hours, weighs, and crude product TLC is done semi-quantitative determination...

Embodiment 2

[0035] Take 500 grams of GBE (containing more than 6% of ginkgolides), heat extract three times with methyl ethyl ketone, each time for 20 minutes, add 1750 ml of methyl ethyl ketone each time, combine the methyl ethyl ketone solution, and use 500 ml of 1% NaHCO 3 The aqueous solution was washed once and then washed once with 1% NaCl, and the washing solution was extracted once again with methyl ethyl ketone, all the methyl ethyl ketone was combined, concentrated under reduced pressure, and dried in vacuum to obtain a residue. The following is the same as in Example 1.

Embodiment 3

[0037] Example 3:

[0038] Take 500 grams of GBE (containing more than 6% ginkgolide), dissolve it with 10% ethanol, extract the ethanol solution three times with chloroform or dichloromethane or dichloroethane, combine the extracts, concentrate under reduced pressure to obtain a residue, the residue Dissolve in ethanol, decolorize the solution through an alumina column, concentrate the obtained ethanol solution to a small volume under reduced pressure, add hot water to dilute, place the dilute alcohol solution to precipitate crystals and filter to obtain a crude product, then purify by recrystallization, recrystallization and Example 1 same.

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Abstract

A process for preparing ginkgolide from ginkgo extract includes such steps as extracting in liposoluble solvent, treating with weak alkali, water washing, concentrating, thermally dissolving it in low-grade alcohol, crystallizing to form semifinished product, thermally dissolving it in alcohol, decolouring with alumina or activated carbon column, concentrating, recrystallizing and vacuum drying.

Description

technical field [0001] The invention relates to the extraction and separation of Chinese herbal medicines, more specifically to the production process of ginkgolides. Background technique [0002] Since the early 1960s, scientists have begun to study ginkgolides, including basic research such as separation and purification, and determination of structures. Ginkgo biloba extract (GBE) was launched in the mid-1970s, and food and health food manufacturers all over the world devoted themselves to the development of Ginkgo biloba with great enthusiasm. The representative one is to prepare Ginkgo biloba extract by solvent extraction method, such as Germany Schwabe, Flaschman pharmaceutical factory, mainly dry ginkgo leaf powder, 60% acetone extraction, pressure filtration, filtrate with CCl 4 Degrease, the acetone aqueous layer is saturated with ammonium sulfate, extracted with methyl ethyl ketone, the extract is concentrated under reduced pressure and made into a certain concent...

Claims

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Application Information

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IPC IPC(8): C07D493/22
Inventor 殷梦龙陈仲良
Owner SHANGHAI INST OF MATERIA MEDICA CHINESE ACAD OF SCI