High efficiency separation and purification method of camptothecine

A technology for separation and purification of camptothecin, which is applied in the fields of organic chemistry, pharmaceutical formulations, and medical preparations containing active ingredients, etc. It can solve the problems of hidden dangers of product safety, difficult removal of impurities, increase of production costs, etc. High efficiency, good extraction effect and small sewage discharge

Inactive Publication Date: 2009-03-25
CHENGDU PUSH BIOLOGICAL TECH
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AI Technical Summary

Problems solved by technology

At present, the purity of domestic products can reach 98%, but the content of its related impurities 10-hydroxycamptothecin, 20-vinylcamptothecin and 9-methoxycamptothecin is often greater than 0.5%. The synchronous reaction of tree alkali produces corresponding impurities in downstream products, and these impurities are not easy to remove, causing hidden dangers to product safety
The refining and purification of downstream products requires a large amount of organic reagents and tedious process operations, which undoubtedly increases the production cost

Method used

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  • High efficiency separation and purification method of camptothecine
  • High efficiency separation and purification method of camptothecine
  • High efficiency separation and purification method of camptothecine

Examples

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Embodiment 1

[0027] A high-efficiency separation and purification method for camptothecin, characterized in that it is carried out according to the following process steps:

[0028] A. Extraction of camptothecin crude product: crush 3000kg camptothecin fruit into coarse powder, and put it into a volume of 6m 3 In the extraction tank, the aqueous methanol solution with a pH value of 9 and a concentration of 70% by volume was used for cyclic extraction for 3 times. For the first time, 8000L of solvent was added, and the extraction time was 8 hours; for the second time, 7000L of solvent was added, and the extraction time was 6 hours; for the third time, 6000L of solvent was added, and the extraction time was 4 hours. The extracts were combined and single-effect concentrated at 70°C to recover methanol. Concentrated hydrochloric acid was added to the concentrated solution to adjust the pH value to neutrality, and then extracted three times with 2000L chloroform, the chloroform phase was conce...

Embodiment 2

[0033] A method for separating and purifying camptothecin, characterized in that it is carried out according to the following processing steps:

[0034] A. Extraction of camptothecin crude product: crush 3000kg camptothecin leaves into coarse powder, and put it into a volume of 6m 3 In the extraction tank, use 80% sodium hydroxide solution to adjust the pH value to 9, and the methanol aqueous solution whose volume ratio concentration is 70% is cyclically extracted for 3 times. For the first time, 8000L of solvent was added, and the extraction time was 8 hours; for the second time, 7000L of solvent was added, and the extraction time was 6 hours; for the third time, 6000L of solvent was added, and the extraction time was 4 hours. The extracts were combined and single-effect concentrated at 70°C to recover methanol. Concentrated hydrochloric acid was added to the concentrated solution to adjust the pH value to neutrality, and then extracted three times with 2000L chloroform, the...

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Abstract

The invention discloses a method for extracting and separating camptothecin from the tissues of a camptotheca, such as fruits, leaves and the like, which comprises the steps of: A. the extraction of camptothecin crude products; B. the preparation of semi-finished products by the separation and purification of the camptothecin crude products; and C. the preparation of products by the concentration and crystallization of the camptothecin semi-finished products. The invention can improve the content of the camptothecin to more than 99 percent, reduce the contents of single related impurities, such as 10-hydroxycamptothecine, 20-ethenylcamptothecin and 9-anisylcamptothecin and the like, to less than 0.1 percent, and has the advantages of high yield, large production, low cost, small pollution and being suitable for industrial production.

Description

technical field [0001] The invention relates to a method for separating and purifying active ingredients of plant monomers, which belongs to the technical field of medicine. Specifically, the invention relates to a method for extracting and separating camptothecin from tissues such as camptothecin fruits and leaves. Background technique [0002] Camptotheca acuminata Decne. is an ancient plant of the blue fruit family. It is a unique plant in my country and has a close relationship with Davidia involucrata. Its secondary metabolite camptothecin is one of the known natural medicines with broad-spectrum anti-tumor activity. one. Camptothecin (CPT) is a pale yellow flaky crystal with the molecular formula C 20 h 16 N 2 o 4 , the molecular weight is 348.36, and the structural formula is as follows: [0003] [0004] Camptothecin [0005] The anti-tumor activity of camptothecin has been recognized all over the world, but its side effects are also more obvious. Nowadays, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22A61K36/185
Inventor 张黎杨兵董维臻夏柯
Owner CHENGDU PUSH BIOLOGICAL TECH
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