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Separation and purification method of bilobalide C

A ginkgolide, separation and purification technology, applied in the direction of organic chemistry and the like, can solve the problems of complex component structure, low purity, complex process, etc., and achieve the effects of improving separation efficiency, production safety, and simple operation.

Active Publication Date: 2013-11-20
SHANGHAI SINE PROMOD PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because ginkgolides have unique pharmacological effects, and these components are only found in one plant of Ginkgo biloba, the structure of this component is complex, and it is extremely difficult to synthesize artificially. Therefore, the extraction of ginkgo leaves has become the main source of ginkgolides. source
There are many reports on the extraction and separation methods of ginkgolides, but the common problems are complicated process, time-consuming and laborious, the yield of ginkgolides is not high, and the purity is not high
Chinese invention patent "Method for Extracting and Separating Ginkgolide C from Ginkgo Leaf" (patent application number 200710050239.X) uses silica gel column chromatography to separate ginkgolide C. The disadvantage of this method is that silica gel cannot be recycled and reused. A large number of organic solvents are eluted, which is unfavorable for industrialized production. Therefore, it is necessary to further improve the extraction and separation method of ginkgolide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Suspend 1 g of ginkgo biloba extract (EGB) (commercially available, total ginkgo lactone content ≥ 6%) in 10 mL of water, extract three times with ethyl acetate, 10 mL each time, extract the solution at 60 °C to recover the solvent under reduced pressure, and extract Heat at 60°C and dissolve in 20mL water, use 50mL MCI-GEL resin for adsorption, the adsorption time is 0.5h, first use 10% ethanol to elute 2BV to remove impurities, then use 30% ethanol to elute resin 2BV, eluate in Evaporate to dryness under reduced pressure at 60°C to obtain crude ginkgolide C, recover the solvent, add 50% ethanol (1.5mL), heat to dissolve at 60°C, place in the refrigerator for 12h, precipitate crystals, repeat recrystallization twice, and use purified water (1mL) The crystals were washed 3 times, heated and dried under vacuum at 65°C to obtain ginkgolide C (16 mg, the content detected by HPLC-ELSD was 98.3%).

Embodiment 2

[0028] Suspend 2 g of ginkgo biloba extract (EGB) (commercially available, with total ginkgo lactone content ≥ 6%) in 20 mL of water, extract three times with ethyl acetate, 20 mL each time, extract the solution at 60 °C to recover the solvent under reduced pressure, and extract Heat at 60°C and dissolve in 40mL of water, and use 70mL of MCI-GEL resin for adsorption. The adsorption time is 2h. Dry the crude product of ginkgolide C, recover the solvent, add 40% ethanol (2.5mL), heat and dissolve at 60°C, place in the refrigerator for 24h, precipitate crystals, repeat recrystallization twice, wash the crystals with purified water three times, and vacuum at 80°C Heated and dried to obtain ginkgolide C (29 mg, HPLC-ELSD detection content: 99.0%).

Embodiment 3

[0030] Take 300g of dried ginkgo leaves (commercially available), crush them, and extract three times under reflux with 80% ethanol. The amount of solvent used is 2.4L, 1.5L and 1.5L in sequence, and each extraction is 2h. , filter, put the filtrate on a macroporous adsorption resin D101 column, wash the column with purified water (1000mL) to remove impurities, and elute with 70% ethanol (2000mL) until the color of the eluate becomes light, and the eluate is concentrated and dried under reduced pressure at 60°C to obtain Ginkgo biloba Leaf extract (6g), the extract was extracted three times with ethyl acetate, 150mL each time, the extraction solution was evaporated to dryness under reduced pressure at 60°C to recover the solvent, the extract was heated and dissolved at 60°C in 20mL water, and processed with 70mL MCI-GEL resin Adsorption, the adsorption time is 1h, first use 10% ethanol to elute 3BV to remove impurities, then use 30% ethanol to elute 1.5BV of resin, the eluate i...

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Abstract

The invention discloses a separation and purification method of bilobalide C, which comprises the steps that an extract of ginkgo biloba is taken and extracted by an organic solvent; the extract is treated by MCI-GEL CHP (Cumene Hydroperoxide) adsorbent resin, subjected to impurity removal and eluted; an eluant is subjected to pressure reduction solvent recovery till dryness; 10-90% ethanol is added, heated, dissolved, refrigerated and kept for 12-48h; crystals are separated out, and subjected to suction filtration; crystallization is performed repeatedly; and the crystals are washed by purified water and dried to form the bilobalide C with the purity capable of reaching above 98%. According to the method, a menstruum for separating and purifying the bilobalide C is simple and easy to obtain, and used equipment is conventional equipment, so that the method is simple to operate, less in energy consumption and low in cost; and nontoxic adsorbent absorption and ethanol desorption are adopted, so that the method is safe in production and pollution-free, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the preparation of traditional Chinese medicine, in particular to a method for separating and purifying ginkgolide C. Background technique [0002] Ginkgo biloba contains a variety of active ingredients, mainly flavonoids, terpene lactones, organic acids, alkylphenols and alkylphenolic acids, steroidal compounds, trace elements, etc. At present, it is known that the medicinal ingredients in Ginkgo biloba are mainly ginkgo flavonoids and ginkgolides. Since ancient times, there have been records of Ginkgo biloba used as medicine and food therapy. Among them, "The Essentials of Materia Medica" mentioned that Ginkgo biloba can "return to the lung meridian, restrain the lungs and relieve asthma, benefit the heart and relieve pain". Modern pharmacological studies have found that ginkgolides have unique physiological effects and therapeutic value, and ginkgolides are strong platelet activating factor (PAF) antagonists. [0003] Plat...

Claims

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Application Information

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IPC IPC(8): C07D493/20
Inventor 肖志勇于垂亮周力军吕署一蒋俊
Owner SHANGHAI SINE PROMOD PHARMA
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