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Preparation method for ginkgolide C

A technology of ginkgolide and ginkgo leaf is applied in the field of preparation of ginkgolide C, which can solve the problems of low yield and purity, and achieve the effects of high purity and high yield

Inactive Publication Date: 2012-05-23
SHANGHAI INST OF PHARMA IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to provide a preparation method of ginkgolide C in order to overcome the defect that the yield and purity are very low in the existing extraction and separation method of ginkgolide C

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Take 3.4kg of sun-dried ginkgo leaves (the content of ginkgolide C is 0.1%), wash once with water, soak and extract with 17L aqueous solution containing 80% ethanol at 60°C for 2h, centrifuge to get the supernatant, and repeat this operation twice , Combine the two supernatants, remove the ethanol by rotary evaporation at 35°C, and obtain the concentrated solution of the alcohol extract.

[0044] Adjust the pH of the above concentrate to 4 with hydrochloric acid, extract twice with ethyl acetate of 1 / 2 the volume of the concentrate each time, discard the raffinate after extraction, add distilled water with a pH of 2 to 5 into the extract, shake After mixing, the water phase was discarded, and the ester phase was rotary evaporated at 30°C until the ethyl acetate was completely removed; then the crude ginkgolide C was dissolved in an aqueous solution containing 10% ethanol, and its pH was adjusted to 2.5 with hydrochloric acid.

[0045] Take the pretreated macroporous ads...

Embodiment 2

[0048] Get 4.1kg of sun-dried ginkgo leaves (the content of ginkgolide C is 0.1%), wash once with water, soak and extract with 20.5L aqueous solution containing 50% ethanol at 70°C for 2h, centrifuge to get the supernatant, repeat this operation twice The two supernatants were combined, and the ethanol was removed by rotary evaporation at 35°C to obtain a concentrated solution of the ethanol extract.

[0049] Adjust the pH of the concentrated solution to 3 with hydrochloric acid, extract twice with ethyl acetate of 1 / 2 the volume of the concentrated solution each time, discard the raffinate after extraction, add distilled water with a pH of 2 to 5 into the extracted phase, shake After mixing, the water phase was discarded, and the ester phase was rotary evaporated at 30°C until the ethyl acetate was completely removed; then the crude ginkgolide C was dissolved in an aqueous solution containing 10% ethanol, and its pH was adjusted to 2.5 with hydrochloric acid.

[0050] Take th...

Embodiment 3

[0053] Take 3.8kg of sun-dried ginkgo leaves (the content of ginkgolide C is 0.1%), wash once with water, soak and extract with 19L aqueous solution containing 60% ethanol at 70°C for 2h, centrifuge to get the supernatant, and repeat this operation twice , Combine the two supernatants, remove the ethanol by rotary evaporation at 35°C, and obtain the concentrated solution of the alcohol extract.

[0054] Adjust the pH of the above concentrate to 4 with hydrochloric acid, extract twice with 1 / 2 volume of ethyl acetate each time, discard the raffinate after extraction, add distilled water with a pH of 2 to 5 into the extract, shake and mix and discard Remove the water phase, and rotate the ester phase at 30°C until the ethyl acetate is completely removed; then dissolve the crude ginkgolide C with an aqueous solution containing 15% ethanol, and adjust its pH to 3 with hydrochloric acid.

[0055] Take the pretreated macroporous adsorption resin NM PS100 (resin pretreatment step: wa...

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PUM

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Abstract

The invention discloses a preparation method for ginkgolide C. The method is characterized by comprising the step of carrying out column chromatographic separation on a crude extract of ginkgo biloba by using a macroporous reverse-phase adsorption resin, wherein, parameters of the macroporous reverse-phase adsorption resin are that a particle size is 50 to 100 mu m, bore diameter is 90 to 110 A and a resin framework is polystyrene-divinylbenzene. The preparation method provided in the invention enables high product yield to be obtained and product purity to be high.

Description

technical field [0001] The invention relates to a preparation method of ginkgolide C. Background technique [0002] Ginkgo biloba L. is a plant of the genus Ginkgo in the Ginkgo family. It appeared about 200 million years ago. It was nearly extinct during the Ice Age and only survived in my country. It was called a "living fossil" by Darwin. With the in-depth research on Ginkgo biloba, it has been proved that the active ingredients of Ginkgo biloba are mainly flavonoids and lactones. Among them, the lactone compounds are: ginkgolide A (BN52020), ginkgolide B (BN52021), ginkgolide C (BN52022), ginkgolide M (BN52023), ginkgolide J (BN52024) and bilobalide . Studies have shown that ginkgolides are strong platelet-activating factor (platelet-activating factor, PAF) receptor antagonists. Their unique pharmacological effects and therapeutic value have aroused great interest in the pharmaceutical industry worldwide. [0003] With the gradual clarification of effective medicinal...

Claims

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Application Information

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IPC IPC(8): C07D493/22
Inventor 李继安郭瑞峰卢亮
Owner SHANGHAI INST OF PHARMA IND
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