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Separation and purification method for bilobalide monomers in ginkgo leaf extract

A technology of ginkgo lactone and ginkgo biloba leaves, applied in the direction of organic chemistry and the like, can solve the problems of difficulty in separation and purification of ginkgo lactone, and achieve the effects of high comprehensive utilization value, convenient operation, and efficient separation and selectivity.

Inactive Publication Date: 2015-06-10
XUZHOU JIYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a method for the separation and purification of bilobalide monomer in Ginkgo biloba extract, the method is easy to operate, low in cost, the purity can reach more than 95%, the product recovery rate is high, and it solves the problem of difficult separation and purification of bilobalide problem, providing a simple and effective method for large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: Get 200 grams of Ginkgo biloba extract (containing about 6 grams of bilobalide), add 1600 ml of water and 400 ml of ethyl acetate, and stir to dissolve. Extract with 1000ml ethyl acetate each time, extract 3 times, and combine the ethyl acetate extracts. Concentrate the extract to recover ethyl acetate, add water and concentrate again, settle overnight, and precipitate most of ginkgolide A, ginkgolide B and ginkgolide C. The mother liquor containing bilobalide was adjusted to 5%-10%, precipitated at room temperature for 2-4 hours, filtered with suction, and the filtrate was extracted with a mixed solution of ethyl acetate and petroleum ether for 3 times, 400-600mL each time, and the light phase was concentrated to dryness. Then heat and dissolve with 300-400mL 15%-30% ethanol at 60°C, let stand overnight, and filter. Put the filtrate on a polyamide resin column, the resin volume is 100-200mL, 200-400mL10-30% ethanol is analyzed, the column effluent and th...

Embodiment 2

[0022] Embodiment 2: Get 4 kilograms of Ginkgo biloba extract (containing about 120 grams of bilobalide), add 32L of water and 8L of ethyl acetate, and stir to dissolve. Extract each time with 20L ethyl acetate, extract 3 times, and combine the ethyl acetate extracts. Concentrate the extract to recover ethyl acetate, add water and concentrate again, settle overnight, and precipitate most of ginkgolide A, ginkgolide B and ginkgolide C. The mother liquor containing bilobalide was adjusted to 5%-10% ethanol, precipitated at room temperature for 2-4 hours, filtered with suction, and the filtrate was extracted 3 times with a mixed solution of ethyl acetate and petroleum ether, 8-12 LL each time, and the light phase was concentrated to dryness. Then heat and dissolve with 6-8L 15%-30% ethanol at 60°C, let it stand overnight, and filter. Put the filtrate on a polyamide resin column, the volume of the resin is 2-4L, and analyze with 4-8L of 10-30% ethanol, combine the effluent from t...

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PUM

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Abstract

The invention relates to a separation and purification method for bilobalide monomers in a ginkgo leaf extract. The separation and purification method comprises the following steps: by taking the ginkgo leaf extract as a raw material, performing extraction and pretreatment, separating polyamide resin, then purifying with a PRP512C chromatographic packing, and finally performing recrystallization to obtain the bilobalide monomers with the purity of 95% or more, wherein the yield of bilobalide is 80% or more. A method for purifying the bilobalide monomers, which is simple and easy to operate, is established.

Description

technical field [0001] The invention relates to a method for separating ginkgolide from ginkgo leaf extract, in particular to a method for separating bilobalide from ginkgo leaf extract. Background technique [0002] Ginkgo Ginkgo L. is the native plant of our country. Ginkgo biloba extracts are widely used at home and abroad to prevent and treat diseases such as cerebrovascular and cardiovascular system dysfunction. The functional components of Ginkgo biloba mainly include flavonol glycosides, bilobalide and ginkgolides A, B, and C. Among them, bilobalide has the effect of treating neurological diseases, and at the same time has a nutritional effect on neurons and nerve tissues, and has a protective effect on glutamate-induced excitotoxic nerve damage. For the treatment of neurological diseases, Alzheimer's disease and myelopathy, anti-aging and so on. However, there is little difference in solubility between bilobalide and flavonoids and colloids in Ginkgo biloba extract...

Claims

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Application Information

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IPC IPC(8): C07D493/20
CPCC07D493/20
Inventor 蒋永红李新晴李五洲曹礼群张艳曹如
Owner XUZHOU JIYUAN PHARMA
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