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High efficiency separation purification method of ginkgolide A, B, C, J and bilobalide monomer

A technology of ginkgolide and bilobalide, which is applied in medical raw materials derived from Ginkgo biloba, organic chemistry, etc., can solve the problems of difficult product quality and quantity to meet market demand, large consumption of reagents, low product yield, etc., and achieve quality Easy to control, avoid blindness, high yield effect

Inactive Publication Date: 2009-03-25
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, traditional methods such as repeated silica gel column chromatography are used to separate and purify ginkgolide monomers at home and abroad. The quality and quantity of the products are difficult to meet the market demand, and the consumption of reagents is large, and the yield of products is low, resulting in high prices for such products.

Method used

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  • High efficiency separation purification method of ginkgolide A, B, C, J and bilobalide monomer
  • High efficiency separation purification method of ginkgolide A, B, C, J and bilobalide monomer
  • High efficiency separation purification method of ginkgolide A, B, C, J and bilobalide monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A high-efficiency separation and purification method of ginkgolides A, B, C, J and bilobalide monomer, characterized in that it is carried out according to the following process steps:

[0029] a. Ginkgo biloba extract to remove ginkgolic acid: take 1Kg of ginkgo biloba extract, add 10L ethanol solution with a concentration of 40% by volume, heat and stir at 50°C to dissolve, let stand for 2h, pour out the supernatant, and pour it into the supernatant Add 6L of petroleum ether (boiling range 60-90°C), fully shake for extraction, let stand to separate layers, and separate liquids. Do this 3 times. The petroleum ether phase recovers petroleum ether, and the residue is discarded; the water phase proceeds to step b.

[0030] b. Obtaining total ginkgo lactones: Concentrate the aqueous phase obtained in step a at 60°C under reduced pressure to recover 2L of organic reagents, add 6L of ethyl acetate to the remaining aqueous liquid, fully shake and extract, let stand to separa...

Embodiment 2

[0036] A high-efficiency separation and purification method of ginkgolides A, B, C, J and bilobalide monomer, characterized in that it is carried out according to the following process steps:

[0037] a. Ginkgo biloba extract to remove ginkgolic acid: take 500 g of ginkgo biloba extract, add 5 L of ethanol solution with a concentration of 50% by volume, heat and stir at 45°C to dissolve, let stand for 2 hours, pour out the supernatant, and pour it into the supernatant Add 3L of petroleum ether (boiling range 60-90°C), fully shake and extract, let stand to separate the layers, and separate the liquids. Do this 3 times. The petroleum ether phase recovers petroleum ether, and the residue is discarded; the water phase proceeds to step b.

[0038] b. Obtaining total ginkgo lactones: Concentrate the aqueous phase obtained in step a at 60°C under reduced pressure to recover 1.5L of organic reagents, add 2.5L of ethyl acetate to the remaining aqueous liquid, fully shake and extract, ...

Embodiment 3

[0044] A high-efficiency separation and purification method of ginkgolides A, B, C, J and bilobalide monomer, characterized in that it is carried out according to the following process steps:

[0045] a. Ginkgo biloba extract to remove ginkgolic acid: take 1500 g of ginkgo biloba extract, add 14 L of ethanol solution with a concentration of 45% by volume, heat and stir at 45 ° C to dissolve, let stand for 2 hours, pour out the supernatant, and pour it into the supernatant Add 8L of petroleum ether (boiling range 60-90°C), fully shake for extraction, let stand to separate the layers, and separate the liquids. Do this 3 times. The petroleum ether phase recovers petroleum ether, and the residue is discarded; the water phase proceeds to step b.

[0046] b. Obtaining total ginkgo lactones: Concentrate the aqueous phase obtained in step A at 60°C under reduced pressure to recover 3L of organic reagents, add 8L of ethyl acetate to the remaining aqueous liquid, fully shake and extrac...

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Abstract

The invention discloses a separating and purifying method of ginkgolides A, B, C and J and bilobalide monomers, which comprises the following processing steps: a. ginkgoic acid is removed from the extractive of ginkgo leafs; b. the total lactones of ginkgo is obtained; c. the preparation solution of the total lactones is prepared; d. the high-performance liquid chromatographic separation of the ginkgolides A, B, C and J and the bilobalide monomers in the total lactones is carried out; and e. the preparation solution of the monomers is processed and the product is dried. By using a preparative high-performance liquid chromatographic column to carry out separation and purification and a differential refractive index detector to carry out on-line detection, the invention can synchronously separate and obtain the ginkgolides A, B, C and J and the bilobalide monomers, the purity of which is more than 98 percent, and has the advantages of large preparative scale, high yield, good product quality, low cost and being suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating and purifying monomeric active ingredients in plants, belonging to the technical field of medicine. Specifically, the invention relates to a method for separating high-purity ginkgolides A, B, C, J and Ginkgolides from ginkgo leaf extracts. A method for bilobalide monomer, and a high performance liquid chromatography method for ginkgolides A, B, C, J and bilobalide monomer. Background technique [0002] Ginkgo biloba L. is a unique relic plant in China. "Chinese Pharmacopoeia" 2005 edition contains ginkgo leaves, ginkgo leaf extracts and ginkgo leaves, which have the effects of astringing the lungs, relieving asthma, promoting blood circulation and removing blood stasis, and relieving pain , for cough and asthma due to lung deficiency, coronary heart disease, angina pectoris, hyperlipidemia, etc. Ginkgo biloba mainly contains active chemical components such as flavonol glycosides and terpenoid lactones....

Claims

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Application Information

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IPC IPC(8): C07D493/22C07D493/18A61K36/16
Inventor 张黎杨兵董维臻夏柯
Owner CHENGDU PUSH BIOLOGICAL TECH
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