Method for separating and purifying paclitaxel industrially

A technology for separation and purification of paclitaxel, applied in the direction of organic chemistry, etc., can solve the problems of increasing the production cost of isolating paclitaxel, restricting industrialized large-scale production, reducing the yield of target paclitaxel, etc., achieving low production costs, reducing industrial production, and avoiding changes Effect

Active Publication Date: 2011-10-19
HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cumbersome operation steps not only reduce the yield of the target paclitaxel and increase the production cost, but also only one product of paclitaxel can be obtained as a result of separation, and the cephalomannine after the structure change can only be discarded as waste, which wastes resources and pollutes the environment
Although reversed-phase column chromatography does not need to change the chemical structure of the separated object, in practical application, this method needs to use a special reversed-phase column silica gel, and its market price is as high as 500,000 yuan / kg
In industrial production, at least 50 kg of reversed-phase column silica gel will be used to separate 1 kg of paclitaxel, and the cost of reversed-phase column silica gel alone will be 25 million yuan, which greatly increases the production cost of separating paclitaxel and limits its industrial scale. mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A sample with a paclitaxel content of 70% was taken as a raw material, and the weight ratio of the raw material to silica gel was 2:100. The raw material was dissolved in dichloromethane for later use. The mobile phase of the quaternary system is n-hexane: dichloromethane: methanol: triethylamine volume ratio = 3:6:2:2, 200-300 mesh silica gel as the stationary phase. The wet method is used to load the column. After the sample is loaded, the column volume is flushed with dichloromethane solvent and then separated with the prepared mobile phase. After 1.4 column volumes of the mobile phase were flushed, paclitaxel C began to flow out, followed by cephalomannine, and after 0.3 column volumes, single paclitaxel flowed out, and paclitaxel could be completely separated after 2 column volumes , Paclitaxel with a purity of more than 90% after one elution accounted for 85%. The paclitaxel effluent with a purity of 30% to 90% was combined and eluted twice. (The separation pro...

Embodiment 2

[0021] A sample with a paclitaxel content of 60% was taken as a raw material, and the weight ratio of the raw material to silica gel was 1.5:100. The raw material was dissolved in dichloromethane for later use. The mobile phase of the five-component system is n-hexane: dichloromethane: acetone: triethylamine: ethyl acetate volume ratio = 6:3:1:1:1.5, and 200-300 mesh silica gel is used as the stationary phase. The wet method is used to load the column. After the sample is loaded, the column volume is flushed with dichloromethane solvent and then separated with the prepared mobile phase. After flushing the mobile phase for 1.7 column volumes, paclitaxel C began to flow out, followed by cephalomannine, and after 0.5 column volumes, single paclitaxel flowed out, and paclitaxel could be completely separated after 2 column volumes , Paclitaxel with a purity of more than 90% after one elution accounted for 75%. The paclitaxel effluent with a purity of 30% to 90% was combined and e...

Embodiment 3

[0023]A sample with a paclitaxel content of 50% was taken as a raw material, and the weight ratio of the raw material to silica gel was 2:100. The raw materials were dissolved in chloroform for later use. The mobile phase of the five-component system is n-hexane: chloroform: acetone: diethylamine: ethyl acetate volume ratio = 4:3:1:1:1.5, and 200-300 mesh silica gel is used as the stationary phase. The wet method is used to load the column. After loading the sample, rinse the column volume with chloroform solvent for 2 column volumes and then separate with the prepared mobile phase. After the mobile phase was flushed for 2 column volumes, paclitaxel C began to flow out, followed by cephalomannine, and after 0.5 column volumes, single paclitaxel flowed out, and paclitaxel could be completely separated after 2.5 column volumes , paclitaxel with a purity of more than 90% after one elution accounted for 66.7%. The paclitaxel effluent with a purity of 30% to 90% was combined and ...

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PUM

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Abstract

The invention discloses a method for separating and purifying paclitaxel industrially and efficiently, and belongs to the field of the separation and purification of compounds. In the method, the paclitaxel is separated by column chromatography, namely the paclitaxel is separated and purified by taking a combination of any three or four of compounds of alkane having 1 to 10 carbon atoms, chlorohydrocarbons, alcohols having 1 to 4 carbon atoms, saturated alkane esters and alkane ketones, and amine compounds as a mobile phase and 200 to 300-mesh ordinary silica gel as a stationary phase by normal phase column chromatography. By selecting a multielement system mixed solvent as the mobile phase, the separation degree of substances which are difficult to separate is increased, and the problem that the paclitaxel cannot be separated from cephalomannine effectively in the conventional separation method is solved. After the paclitaxel is separated and purified by the column chromatography, the purity of paclitaxel crude products serving as raw materials can be improved to be over 98 percent, and according to the condition of the raw materials, the total yield is up to 90 percent only by eluting the paclitaxel crude products once to twice. In the method, the common solvent and silica gel are used, so the cost is low, the method is easy and convenient to operate, the sample volume is large, and industrial production is easy to realize.

Description

technical field [0001] The invention relates to a separation and purification method of paclitaxel, in particular to an industrialized high-efficiency separation and purification method of paclitaxel and cephalomannine, which belongs to the field of compound separation and purification. Background technique [0002] Paclitaxel is a new type of anticancer drug isolated from Taxus genus with a taxane diterpene skeleton. It is also the only drug known to promote microtubule polymerization and stabilize the polymerized microtubules. It has a strong inhibitory effect on most solid tumors, but basically has no effect on normal cells, especially for advanced ovarian cancer, breast cancer, non-small cell lung cancer and Kaposi's sarcoma, with definite curative effect and less side effects. With the further research, the anti-cancer effect of paclitaxel drugs has been more and more widely used, and has now become a first-line anti-cancer drug and a broad-spectrum anti-tumor drug. ...

Claims

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Application Information

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IPC IPC(8): C07D305/14
Inventor 薛宝玉李文锋樊燕鸽赵俊宏曹继红丁奎岭
Owner HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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