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Method for separating and purifying GA, GB and bilobalide from folium ginkgo extractive

A technology for separation and purification of bilobalide, applied in the fields of B, bilobalide, and ginkgolide A, which can solve problems such as complex process routes, and achieve the effects of simple process routes, high product yields, and low production costs

Active Publication Date: 2013-04-17
SUZHOU ZEDAXINGBANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method uses the process route of alcohol extraction-extraction-resin purification-crystallization-silica gel column separation-crystallization and other steps, the process route is complicated, and only GB

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Take 100g of Ginkgo biloba extract (GA content 2.1%, GB content 1.2%, BB2.5%), add 500mL water and stir at 50°C for 30min, then add 500mL ethyl acetate for extraction, extract 5 times, combine the ethyl acetate extracts, Concentrate and dry the ethyl acetate extract to obtain 15.5g of ethyl acetate extract; add 155mL of 70% ethanol to extract at 50°C for 1 hour, filter, and dry the filter cake to obtain 4.4g of insoluble matter and 150mL of alcohol extract; After dissolving 20mL of ethyl acetate, mix the sample with 5g of 100-200 mesh silica gel, then use 200g of 200-300 mesh silica gel column chromatography to separate, elute with a mixed solvent of petroleum ether-ethyl acetate 8:2, collect the eluent in sections, The solvent in the eluate was recovered to obtain 1.8 g (purity: 98.2%) of GA and 1.0 g (purity: 98.5%), respectively. 150 mL of the alcohol extract was concentrated to 40 mL at 60°C under reduced pressure, cooled to 25°C, filtered, the mother liquor was con...

Embodiment 2

[0050] Take 100g of Ginkgo biloba extract (GA content 2.1%, GB content 1.2%, BB2.5%), add 700mL water and stir at 30°C for 30min, then add 1000mL ethyl acetate for extraction, extract 3 times, combine the ethyl acetate extracts, Concentrate and dry the ethyl acetate extract to obtain 16.5g of ethyl acetate extract; add 330mL of 70% ethanol for leaching at 20°C for 1 hour, filter, and dry the filter cake to obtain 4.6g of insoluble matter and 310mL of alcohol extract; After dissolving 20mL of ethyl acetate, mix the sample with 5g of 100-200 mesh silica gel, then use 200g of 200-300 mesh silica gel column chromatography to separate, elute with a mixed solvent of petroleum ether-ethyl acetate 3:7, collect the eluent in sections, The solvent in the eluate was recovered to obtain GA1.7g (purity 98.1%) and GB0.98g (purity 98.3%), respectively. 310mL of the alcohol extract was concentrated to 100mL under reduced pressure at 60°C, cooled to 25°C, filtered, and the mother liquor was co...

Embodiment 3

[0052] Take 100g of Ginkgo biloba extract (GA content 2.1%, GB content 1.2%, BB2.5%), add 1000mL water and stir at 20°C for 30min, then add 1000mL ethyl acetate for extraction, extract 4 times, combine the ethyl acetate extracts, Concentrate and dry the ethyl acetate extract to obtain 16.0 g of ethyl acetate extract; add 320 mL of 30% ethanol to extract at 50 ° C for 1 hour, filter, and dry the filter cake to obtain 4.8 g of insoluble matter and 300 mL of alcohol extract; After dissolving 20mL of ethyl acetate, mix the sample with 5g of 100-200 mesh silica gel, and then use 200g of 200-300 mesh silica gel column chromatography to separate and elute with a mixed solvent of petroleum ether-ethyl acetate 4:6, and collect the eluent in sections. The solvent in the eluate was recovered to obtain 1.75 g (purity: 98.0%) of GA and 1.05 g (purity: 98.1%) of GB, respectively. 300mL of the alcohol extract was concentrated to 70mL under reduced pressure at 60°C, cooled to 25°C, filtered, ...

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Abstract

The invention discloses a method for separating and purifying GA (Ginkgolide A), GB (Ginkgolide B) and bilobalide from a folium ginkg extractive. The method comprises the following steps that 1), ethyl acetate is adopted for extraction; 2), a lower alcohol-water mixed solvent is adopted for leaching; an alcohol leaching extraction solution and an undissolved substance are obtained; 3), the undissolved substance is subjected to silica gel column chromatography separation to form GA and GB; and 4), the alcohol leaching extraction solution is concentrated till no alcohol exists, cooled and filtered; a mother solution is concentrated to dryness, and then subjected to crystallization with 30-35% of methanol for 3-5 times; and bilobalide is obtained. The method for separating and purifying GA, GB and bilobalide is simple in process route and is suitable for industrial production. The purity of GA, GB and bilobalide obtained by separation and purification is greater than 98%; transfer rates of GA, GB and bilobalide are greater than 80%; the yield is high; the production cost is low.

Description

technical field [0001] The invention relates to a method for ginkgolides A, B and bilobalide, in particular to a method for separating and purifying GA, GB and bilobalide from ginkgo leaf extract. Background technique [0002] Ginkgo biloba extract plays an important role in promoting platelet activation in the circulatory system, anti-oxidation, anti-aging function, anti-senile dementia and eye retinopathy, etc. Transgender drugs. According to incomplete statistics, as of August 2010, the State Food and Drug Administration has issued more than 140 approval documents for the production of ginkgo biloba extract drugs and compound preparations, and there are more than 100 manufacturers. In today's world market, the annual sales of ginkgo biloba products have reached more than 6 billion US dollars, and it has become the global champion variety of herbal medicines. Ginkgo biloba preparations have become the leading varieties for the treatment of cardiovascular and cerebrovascul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/22C07D493/20
Inventor 栾连军刘雪松谈满良荆海英吴永江陈勇王龙虎
Owner SUZHOU ZEDAXINGBANG MEDICAL TECH
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