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Preparation method of larotaxel

A kind of technology of rallotase and crude products, which is applied in the field of medicine to achieve the effect of easy control and simplified process technology

Inactive Publication Date: 2019-01-15
江苏汉邦科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The present invention aims to provide a preparation method of raloxaline, so as to solve the problem that there is no better method for separating and purifying larlotaxel at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Take 100g of the crude product of larlotaxide and ultrasonically dissolve it with 60% acetonitrile aqueous solution to remove tiny solid insolubles and obtain the filtrate as the separated crude product; inject the filtrate into the liquid phase preparative chromatography separation system, and the dynamic axial compression column size is 50×250mm, The stationary phase is silica gel filler, the particle size is 20-45um, the sample loading is 100g, and the mobile phase flow rate is 50ml / min. The volume ratio of mobile phase acetonitrile and water is 55 / 45, and the elution time is 120min. The detection wavelength of the ultraviolet photometric detector used is 230nm, and the components with a retention time of 20-40min are collected, evaporated to dryness, and analyzed by HPLC with a purity of ≥90%.

Embodiment 2

[0013] Take 150g of the crude product of larlotaxide and ultrasonically dissolve it with 60% acetonitrile aqueous solution to remove tiny solid insoluble matter, and obtain the filtrate as the separated crude product; inject the filtrate into the liquid phase preparative chromatography separation system, and the dynamic axial compression column size is 100×250mm, The stationary phase is silica gel packing, the particle size is 20-45um, the sample loading is 150g, the flow rate of the mobile phase is 150ml / min, the volume ratio of acetonitrile and water in the mobile phase is 55 / 45, and the elution time is 120min. The detection wavelength is 230nm, and the components with a retention time of 20-40min are collected, evaporated to dryness, and analyzed by HPLC with a purity of ≥90%.

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Abstract

The invention discloses a preparation method of larotaxel. The method includes: taking acetonitrile and water as the mobile phase, and separating and purifying a larotaxel crude product by a liquid chromatography system to obtain high purity larotaxel. The method provided by the invention has the advantages of simple operation, short cycle, high efficiency, and purity up to 90% or more.

Description

technical field [0001] The invention belongs to the technical field of medicines, and in particular relates to a preparation method of larrotaxed. Background technique [0002] Larotaxel is a protein drug, which mainly stops cell division in the middle of mitosis by inhibiting the polymerization of tubulin. It is a cell cycle-specific drug. The drug not only has stronger anti-tumor activity than paclitaxel and docetaxel, but also has strong anti-multidrug resistance. It is clinically used in patients with metastatic breast cancer who have previously received paclitaxel or docetaxel. Better tolerated and less irritating. At present, there are few studies on the separation and purification methods of raloxataxel, so it is necessary to develop an efficient separation and purification method. Contents of the invention [0003] The present invention aims to provide a preparation method of larrotaxel, so as to solve the problem that there is no better method for separating and...

Claims

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Application Information

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IPC IPC(8): C07D305/14
CPCC07D305/14
Inventor 陈龙陈亮刘大伟
Owner 江苏汉邦科技股份有限公司
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