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Method for directly extracting camptothecin from mappia foetida

A direct technique of camptothecin, applied in the field of extracting antitumor medicinal chemical constituent camptothecin, can solve the problems of difficulty in solvent recovery, low product yield, long time consumption, etc., shorten the extraction time, improve economic benefits, The effect of reducing usage

Inactive Publication Date: 2009-12-09
SHANGHAI LONGXIANG BIO MEDICINE DEV CO LTD
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  • Summary
  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The main deficiency of this method is that the productive rate of camptothecin is too low, only 0.11%; This method adopts the method for soaking in low-temperature solvent to extract, and each time Mabi wood powder needs to be soaked in solvent overnight, so complete the whole extraction process It takes at least one week; in addition, the method requires a large amount of solvent, resulting in a higher cost for the extraction process of camptothecin
Therefore, this method takes a long time, has high cost and low yield, and is not suitable for large-scale production.
[0008] Chinese patent ZL02132721 discloses a method for extracting camptothecin from the unique Chinese involucrata plant Camptothecin, using alcohol (50-70% ethanol) or alkyd as the extraction solvent, through about 8 steps, about It takes 1 week to complete one extraction, and the yield of the product obtained is also low, only 0.04-0.06%
Subsequent purification steps also repeatedly use dichloromethane or chloroform for purification, which will cause a great impact on the environment
[0009] Chinese patent ZL200310111050 also discloses a method for extracting camptothecin from Camptotheca involucrata, a plant unique to China, using ethanol (60-90% ethanol) as the extraction solvent, which also requires multiple complicated steps, about 1 Weeks can complete an extraction, and the yield of the resulting product is also low, only about 0.04%
This method improves the total yield of mabi wood extraction to 0.15%, and shortens the time of extraction, but the whole process of extracting camptothecin using this method must use several pure organic solvents to realize, and the extracted camptothecin The crude resin still needs to be purified through multiple recrystallizations, resulting in product loss and higher production costs
[0011] There are many defects in the above-mentioned prior art. A large number of toxic and harmful organic solvents are used, which makes the recovery of solvents difficult and causes many adverse effects on the environment; the process steps for extracting camptothecin are complicated and too many; the work required for a single extraction The time is too long, usually one week; the final CPT extraction yield is too low, usually no more than 0.05%

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: extraction solvent selects ethanol / water

[0030] Grind the raw material of Mabi wood, weigh 1kg of Mabi wood fine powder into a 10L reaction bottle, add 4L of ethanol / water=3 / 2(v / v) mixed solvent to stir and extract, heat to 70°C, stir and extract for 3h, After the extract was filtered, the resulting residue was further added with 4 L of ethanol / water=3 / 2 (v / v) mixed solvent and stirred at 70° C. for 3 h. After extracting 3 times according to this method, the camptothecin in Mabi wood is basically completely extracted. After the three extracts were combined, the solvent was distilled off under reduced pressure to obtain a crude product of camptothecin, which was recrystallized twice with acetic acid to obtain 1.8 g of camptothecin crystals, with a total yield of 0.18%.

Embodiment 2

[0031] Embodiment 2: methanol / water is selected as the extraction solvent

[0032] Grind the raw material of Mabi wood, weigh 1kg of Mabi wood fine powder into a 10L reaction bottle, add 4L of methanol / water=3 / 2(v / v) mixed solvent to stir and extract, heat to 60°C, stir and extract for 3h, The residue obtained after filtering the extract was further added with 4 L of ethanol / water=3 / 2 (v / v) mixed solvent and stirred at 60° C. for 3 h. After extracting 3 times according to this method, the three extracts were combined, and the solvent was evaporated under reduced pressure to obtain the crude product of camptothecin. After the crude product was recrystallized twice with acetic acid, 0.95 g of camptothecin crystals could be obtained, and the total yield was 0.09 %.

Embodiment 3

[0033] Embodiment 3: extraction solvent selection tetrahydrofuran / water

[0034] Grind the raw material of Mabi wood, weigh 1kg of Mabi wood fine powder into a 10L reaction bottle, add 4L of tetrahydrofuran / water (v / v=3 / 2) mixed solvent to stir and extract, heat to 60°C and then stir and extract for 3h, The residue obtained after filtering the extract was further added to 4 L of tetrahydrofuran / water=3 / 2 (v / v) mixed solvent and stirred at 60° C. for 3 h. Extracted 3 times according to this method, combined the three extracts, and evaporated the solvent under reduced pressure to obtain the crude product of camptothecin, which required 4 times of recrystallization with acetic acid to obtain 0.50 g of camptothecin crystals, with a total yield of 0.05%.

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PUM

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Abstract

The invention relates to a method for directly extracting camptothecin from mappia foetida. A mixed solvent of an organic solvent and water is adopted to directly extract out the camptothecin from the mappia foetida, thereby not only reducing the usage amount of the solvent and simplifying a previous process for extracting various solvents, but also ensuring that the extraction is more complete and improving the total yield of the camptothecin. The extraction is carried out under the condition of 60-70 DEG C, and compared with the previous extraction at room temperature or low temperature, the extraction of the method can ensure that the camptothecin in the mappia foetida can be dissolved in the solvent at a higher speed so as to greatly shorten the extraction time. The method has simple operation, and the total yield of the camptothecin reaches 0.18 percent, thus, compared with the previous extraction process, the method is more suitable for industrial mass production.

Description

technical field [0001] The invention relates to a production method for extracting camptothecin, a chemical component of an antineoplastic drug, in particular to a method for extracting camptothecin by using mabi wood produced in western Hunan as a raw material. Background technique [0002] Camptothecin (CPT) is an alkaloid that was first extracted from the Chinese Nyssaceae (Nyssaceae) plant Camptotheca acuminata by American scientist Wall et al. in 1966. It has a unique anti-tumor effect , but because of its poor water-solubility and fat-solubility, its toxic and side effects are relatively large, which limits its clinical application. In 1985, the research results of Hsiang et al. of John Hopkins University showed that CPT is a specific inhibitor of DNA topoisomerase I (Topo I), and Topo I is a ribozyme of cells, which is related to DNA replication, transcription, It is related to repair and recombination, and it is expressed at any stage of the cell cycle, and it is kn...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22A61K36/185
Inventor 高河勇冯虓韩怡政
Owner SHANGHAI LONGXIANG BIO MEDICINE DEV CO LTD
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