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Method for extracting and separating bilobalide B from ginkgo leaf

A technology for ginkgolide and ginkgo leaf is applied in the field of extraction and separation of ginkgolide B, which can solve problems such as difficulty in extraction and separation, and achieve the effects of low production cost, simple process and high purity

Inactive Publication Date: 2009-04-22
桂林市振达生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ginkgolides mainly include ginkgolides A, B, C, J and M monomers; according to literature reports, there are certain differences in the drug functions of each monomer in ginkgolides. Vascular disease has remarkable curative effect, and bilobalide has unique medicinal effect to treating nervous system disease, in order to improve its medicinal therapeutic effect, must separate and purify each monomer sometimes; Since bilobalide is a sesquiterpene substance, and Esters A, B, C, J, and M are diterpenes, their molecular structures are relatively similar, and their polarity difference is also small, which makes the extraction and separation of each monomer in ginkgolide more difficult

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 1) Get 10 kilograms of ginkgo leaves, use 100 liters of ethanol with a volume concentration of 80% to extract the ginkgo leaves for 1 hour at 50 ° C, and separate the ginkgo leaves with 200 mesh filter cloth; use 60 liters of ethanol with a volume concentration of 55% Extract the ginkgo leaves with ethanol for 1 hour at 70°C, and separate the ginkgo leaves with a 200-mesh filter cloth; then use 50 liters of ethanol with a volume concentration of 25% to extract the ginkgo leaves for 1 hour at 50°C, and use a 200-mesh filter cloth to extract the ginkgo leaves for 1 hour. Ginkgo biloba is separated; the extract obtained from the three extractions is combined, ethanol is recovered, and the extract is concentrated to 100 liters of concentrate;

[0019] 2) Add 100 liters of ethyl acetate to the concentrated solution to extract 3 times, combine the organic phases separated by extraction, recover the organic phase and concentrate to obtain 500 grams of extract;

[0020] 3) Dilu...

Embodiment 2

[0024] 1) Get 50 kilograms of ginkgo leaves, use 400 liters of ethanol with a volume concentration of 60% to extract the ginkgo leaves for 3 hours at 70 ° C, and separate the ginkgo leaves with 200 mesh filter cloth; then use 400 liters of ethanol with a volume concentration of 30% Ethanol extracts the ginkgo leaves for 3 hours at 70°C, and separates the ginkgo leaves with a 200-mesh filter cloth; then uses 300 liters of ethanol with a volume concentration of 10% to extract the ginkgo leaves for 3 hours at 70°C, and uses a 200-mesh filter cloth to extract the ginkgo leaves. Ginkgo biloba is separated; the extract obtained by merging the three extractions is recovered, the ethanol is recovered, and the extract is concentrated to 500 liters of concentrate;

[0025] 2) Add 500 liters of ethyl acetate to the concentrated solution to extract 3 times, combine the organic phases separated by extraction, recover the organic phase and concentrate to obtain 1.5 kg of extract;

[0026] 3...

Embodiment 3

[0030] 1) Get 40 kilograms of ginkgo leaves, use 280 liters of ethanol with a volume concentration of 70% to extract the ginkgo leaves for 1 hour at 70 ° C, and separate the ginkgo leaves with 200 mesh filter cloth; Extract the ginkgo leaves with ethanol for 2 hours at 60°C, and separate the ginkgo leaves with a 200-mesh filter cloth; then use 280 liters of ethanol with a volume concentration of 20% to extract the ginkgo leaves for 2 hours at 70°C, and use a 200-mesh filter cloth to extract the ginkgo leaves. Ginkgo biloba is separated; the extract obtained by merging the three extractions is recovered, the ethanol is recovered, and the extract is concentrated to 400 liters of concentrate;

[0031] 2) Add 400 liters of ethyl acetate to the concentrated solution to extract 3 times, combine the organic phases separated by extraction, recover the organic phase and then concentrate to obtain 1.2 kg of extract;

[0032] 3) Dilute the extract obtained in step 2) with 100 times the v...

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PUM

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Abstract

The invention discloses a method for extracting and separating ginkgolides B from folium ginkgo, which comprises the following steps: 1) taking the folium ginkgo, carrying out extraction by ethanol with different concentrations from high to low, combining extracting solutions, and reclaiming the ethanol to obtain concentrated extracting solution; 2) adding ethyl acetate into the concentrated extracting solution for extraction, reclaiming organic phase and concentrating the extracting solution into extract; 3) diluting the extract obtained in step 2), putting the extract to preferential polar imperforate adsorption resin, washing the preferential polar imperforate adsorption resin by ethanol, reclaiming the ethanol in eluate, and crystallizing by the ethanol to obtain ginkgolides compounds; 4) putting the ginkgolides compound crystal to silica gel column, washing the silica gel column by miscible liquids of normal hexane and ethyl acetate, and collecting eluate to obtain eluate of ginkgolides B; and 5) reclaiming solvent in eluate collected in step 4), and crystallizing the solvent by ethanol to obtain ginkgolides B monomer. The method has the advantages of simple process, low production cost, high purity of products, and easy industrial production.

Description

(1) Technical field: [0001] The invention relates to a method for extracting active ingredients from plants, in particular to a method for extracting and separating ginkgolide B from ginkgo leaves. (two) background technology: [0002] Ginkgo tree, also known as ginkgo tree, is a gymnosperm and is one of the only surviving old tree species of the genus Ginkgo in the family Ginkgoceae. Its leaves and fruits have important medicinal value. The most studied is Ginkgo biloba extract, which includes flavonoids and ginkgolides. There are about 38 kinds of flavonoids, with a total content of 22-27%; ginkgolides include ginkgolide and bilobalide, with a total content of 5.4-6.6%. Ginkgolides mainly include ginkgolides A, B, C, J and M monomers; according to literature reports, there are certain differences in the drug functions of each monomer in ginkgolides. Vascular disease has remarkable curative effect, and bilobalide has unique medicinal effect to treating nervous system dise...

Claims

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Application Information

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IPC IPC(8): C07D493/22A61K36/16A61K127/00
Inventor 孙莉莉罗增桂唐江明李振志
Owner 桂林市振达生物制药有限公司
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