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Separation and purification method of docetaxel

A docetaxel, separation and purification technology, applied in the field of high-efficiency separation and purification of docetaxel, can solve the problems such as the purification method's purity and yield need to be further improved, and achieve stable yield, high yield and mobile phase quantity. saving effect

Pending Publication Date: 2021-10-29
CHANGSHU NANOMICRO BIOTECHNOLOGY CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But the purity and the yield of this purification method need to be further improved

Method used

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  • Separation and purification method of docetaxel
  • Separation and purification method of docetaxel
  • Separation and purification method of docetaxel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1) Take the crude product of docetaxel with a purity of 97%, add dichloromethane to dissolve it, and obtain a docetaxel solution with a concentration of 50 mg / mL; use;

[0040] 2) Use a 50×250mm chromatographic column, UniSil normal phase silica gel (produced by Suzhou Nawei Technology Co., Ltd.) as the chromatographic column filler, and the column volume is 490mL; pre-column pretreatment of the chromatographic column, first use ethyl acetate Ester carries out impurity removal, after using volume ratio is dichloromethane: the mobile phase of ethyl acetate=9:1 balances; Then sample injection, sample liquid is 1) described filtrate; Then adopting volume ratio is dichloromethane: The mixed solution of ethyl acetate=9:1 was used as the mobile phase to elute for 240min, and the flow rate was controlled at 60mL / min;

[0041] 3) The solution of the target peak was collected in sections, and the components meeting the requirements were summarized. After analysis by high perfor...

Embodiment 2

[0044] 1) Take the crude product of docetaxel with a purity of 97%, add dichloromethane to dissolve it, and obtain a docetaxel solution with a concentration of 50 mg / mL; use;

[0045] 2) Use a 50×250mm chromatographic column, UniSil normal phase silica gel (produced by Suzhou Nawei Technology Co., Ltd.) as the chromatographic column filler, and the column volume is 490mL; pre-column pretreatment of the chromatographic column, first use ethyl acetate Esters were used to remove impurities, and then equilibrated with a mobile phase with a volume ratio of dichloromethane:ethyl acetate=8.5:1.5. Then adopting volume ratio is dichloromethane: the mobile phase of ethyl acetate=8.5:1.5 carries out elution 240min, and flow velocity is controlled at 60ml / min;

[0046] 3) Collect the solution of the target peak in sections, summarize the component solutions that meet the requirements, and analyze by high performance liquid chromatography, the purity of docetaxel in the eluent is 99.56%, ...

Embodiment 3

[0048] The difference between this example and Example 1 is that the organic solution for dissolving the docetaxel sample is ethyl acetate, and the others are the same as those in Example 1.

[0049] The solution of the target peak was collected in sections, and the components meeting the requirements were summarized. After analysis by high performance liquid chromatography, the purity of docetaxel in the eluent was 99.51%, and the yield was 95.2%.

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Abstract

The invention provides a separation and purification method of docetaxel. The separation and purification method of docetaxel comprises the following steps: 1) dissolving a docetaxel crude product, and filtering to obtain a docetaxel solution; 2) loading the docetaxel solution obtained in the step 1) into a chromatographic column filled with UniSil microspheres for chromatography, and eluting the docetaxel solution by adopting an organic solvent as a mobile phase; and (3) sectionally collecting the docetaxel solution with the target peak value after chromatography and elution in the step (2), and summarizing the component solutions meeting the requirements to obtain purified docetaxel. The separation and purification method is used for deep purification of docetaxel, the requirement that the total purity is larger than 99.5% can be met only through one-step chromatographic purification, the purification yield is high and stable, meanwhile, the separation method is simple and convenient and can be used for large-scale production, and the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the technical field of medicine purification, and relates to a separation and purification method of docetaxel, in particular to a high-efficiency separation and purification method of docetaxel. Background technique [0002] Docetaxel (docetaxel) has the same effect as paclitaxel (PTX). It is an M-phase cycle-specific drug that promotes the polymerization of tubules into stable microtubules and inhibits their aggregation, thereby significantly reducing the number of tubules. And can destroy the microtubule network structure. In vitro experiments show that it has cytotoxic effect on various mouse and human tumor cell lines, and its antitumor spectrum is wider than that of PTX. [0003] Docetaxel is a paclitaxel derivative synthesized during the structural modification of paclitaxel, which has good bioavailability and less toxic side effects. Docetaxel is a paclitaxel anti-tumor drug, which plays an anti-tumor effect by interf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/14
CPCC07D305/14
Inventor 陶冶王希郁明钧
Owner CHANGSHU NANOMICRO BIOTECHNOLOGY CO LTD
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