Method for highly efficiently extracting paclitaxel from Chinese yew

A technology of yew and paclitaxel, applied in the direction of organic chemistry, can solve the problems of low extraction yield and expensive equipment, achieve high extraction efficiency, reduce the amount of solvent, and meet the requirements of product purity

Active Publication Date: 2015-11-04
贵州玉福临科技开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The technical problem solved by the present invention is to provide a method for efficiently extracting paclitaxel from yew, which effectively sol...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Take 0.5 kg of yew raw material, grind through a 100-mesh sieve, add 5 times the amount of water and 0.1% glacial acetic acid to it, add 0.02% cellulase at room temperature, and place it under ultrasonic (power 50W) Enzymatic hydrolysis for 5 hours. After the enzymatic hydrolysis, an equal volume of ethyl acetate was added, and ultrasonic (power 400W) was extracted for 1 hour. Static filtration, liquid separation, the aqueous phase was extracted 3 times with ethyl acetate, and the organic phases were combined. Ethyl acetate was removed under reduced pressure, and the obtained extract was mixed with an equal mass of neutral alumina, passed through a 200-mesh alumina chromatography column, first eluted with petroleum ether and ethyl acetate to remove fat-soluble impurities, and then mixed with methanol and ethyl acetate The mixture of ester volume ratio was 1:0.3 was eluted, monitored by TLC, and methanol and ethyl acetate fractions were collected. Methanol and ethyl ac...

Embodiment 2

[0035] Take 0.5 kg of yew raw material, grind it through a 100-mesh sieve, add 7 times the amount of water and 0.1% glacial acetic acid to it, add 0.02% cellulase in an environment of 40°C, and place it in an ultrasonic (power 20W) Enzyme hydrolysis for 3 hours. After the enzymatic hydrolysis, an equal volume of chloroform was added, and ultrasonic (500W) extraction was performed for 2 hours. Set aside to filter, separate the layers, extract the aqueous phase with chloroform three times, and combine the organic phases. Chloroform was removed under reduced pressure, and the obtained extract was mixed with an equal mass of neutral alumina, passed through a 200-mesh silica gel chromatography column, first eluted with petroleum ether and ethyl acetate to remove fat-soluble impurities, and then mixed with ethanol and ethyl acetate volume ratio The 1:0.4 mixture was eluted, monitored by TLC, and the fractions of ethanol and ethyl acetate were collected. Ethanol and ethyl acetate w...

Embodiment 3

[0037]Take 1.0 kg of yew raw material, grind it through a 200-mesh sieve, add 5 times the amount of water and 0.1% glacial acetic acid to it, add 0.02% cellulase at room temperature, and place it under ultrasonic (power 20W) Enzymatic hydrolysis for 2 hours. After the enzymatic hydrolysis, an equal volume of ethyl acetate was added, and ultrasonic (power 300W) extraction was performed for 0.5 hours. Static filtration, liquid separation, the aqueous phase was extracted twice with ethyl acetate, and the organic phases were combined. Ethyl acetate was removed under reduced pressure, and the obtained extract was mixed with an equal mass of neutral alumina, passed through a 200-mesh alumina chromatography column, first eluted with petroleum ether and ethyl acetate to remove fat-soluble impurities, and then mixed with methanol and ethyl acetate The mixture of ester volume ratio was 1:0.4 was eluted, monitored by TLC, and the fractions of methanol and ethyl acetate were collected. ...

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Abstract

The invention relates to a method for highly efficiently extracting paclitaxel from Chinese yew. According to the invention, a Chinese yew raw material is ground and sieved using a 100-200 mesh sieve; water with an amount 5-10 times that of ground Chinese yew and 0.1% glacial acetic acid are added, and ultrasonic-assisted enzymolysis is carried out; the obtained material is allowed to stand, and is filtered and separated; ultrasonic-assisted organic solvent extraction is carried out; impurity-removing is carried out through column chromatography; alkaline resin column continuous purification and separation is carried out; and recrystallization is carried out, such that a pure product with a purity higher than 99.3% is obtained. The method provided by the invention has the advantages of simple process steps, low cost, good repeatability, and high product purity.

Description

technical field [0001] The invention relates to a method for efficiently extracting paclitaxel from Taxus chinensis, especially using Taxus chinensis as raw material, after ultrasonic-assisted enzymolysis, column chromatography and basic resin column separation, recrystallization and refining, the extraction efficiency is greatly improved, Reduced production costs. Background technique [0002] Taxus (commonly known as yew, yew) belongs to the Gymnosperm subphylum (Gymnospcrloe), which has long been recorded in Chinese medicine: "Compendium of Materia Medica" records that yew has curative effects on cholera, typhoid, and detoxification. In 1971, American chemist Wani et al. isolated the taxane diterpene compound paclitaxel with high anticancer activity from the bark of the short-leaved yew (T. brevifolia) produced in North America, and found that paclitaxel has a unique anti-tumor effect. Microtubule protein binds to form a stable stable tube bundle, and depolymerizes, stop...

Claims

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Application Information

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IPC IPC(8): C07D305/14
CPCC07D305/14
Inventor 曾发忠
Owner 贵州玉福临科技开发有限公司
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