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Method for separation purification of epothilone by using dynamic axial compression column

An axial compression, epothilone technology, applied in the field of biochemistry, can solve the problems of low purity, serious environmental pollution, large solvent consumption, etc. Simple process and the effect of reducing production costs

Active Publication Date: 2013-09-04
江苏迪沃特仪器设备科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved in the present invention is to provide a method for separating and purifying epothilone with a dynamic axial compression column, which can solve the problem of large solvent consumption and serious environmental pollution when using liquid-liquid extraction technology to extract epothilone in the prior art , and the problem of low purity of epothilones in HPLC detection

Method used

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  • Method for separation purification of epothilone by using dynamic axial compression column
  • Method for separation purification of epothilone by using dynamic axial compression column
  • Method for separation purification of epothilone by using dynamic axial compression column

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Embodiment 1

[0034] A method for separating and purifying epothilone with a dynamic axial compression column, comprising the following steps:

[0035] (1) Mobile phase preparation: prepare normal phase mobile phase with n-hexane and ethyl acetate as the sample normal phase eluent, the volume ratio of n-hexane and ethyl acetate is 80:20; use methanol and water to prepare reverse To the mobile phase, as the reverse phase eluent of the sample, the volume ratio of the methanol and water is 90:10;

[0036] (2) Dissolution and filtration: Dissolve 30 g of crude epothilone with a purity greater than 60% in a mixed solution of n-hexane, ethyl acetate, and isopropanol with a volume ratio of 1:1:1, and use a 0.45 μm organic filter membrane after ultrasonication Filter, and the filtrate is further diluted with the normal phase mobile phase prepared in step (1) to a sample with a concentration of 0.5g / ml;

[0037] (3) Packing of dynamic axial compression column: 960g of 200-800 mesh polar silica gel ...

Embodiment 2

[0044] A method for separating and purifying epothilone with a dynamic axial compression column, comprising the following steps:

[0045] (1) Mobile phase preparation: prepare normal phase mobile phase with n-hexane and ethyl acetate as the sample normal phase eluent, the volume ratio of n-hexane and ethyl acetate is 40:60; use methanol and water to prepare reverse To the mobile phase, as the reverse phase eluent of the sample, the volume ratio of the methanol and water is 70:30;

[0046] (2) Dissolution and filtration: 120 g of crude epothilone with a purity greater than 60% was dissolved in a mixed solution of ethyl acetate and isopropanol with a volume ratio of 3:2, filtered with a 0.45 μm organic filter membrane after ultrasonication, and the filtrate was further used Dilute the normal phase mobile phase prepared in step (1) to a sample with a concentration of 0.3g / ml;

[0047] (3) Dynamic axial compression column packing: 4000g of 200-800 mesh polar silica gel filler and...

Embodiment 3

[0054] A method for separating and purifying epothilone with a dynamic axial compression column, comprising the following steps:

[0055] (1) Mobile phase preparation: prepare the normal phase mobile phase with n-hexane and ethyl acetate as the sample normal phase eluent, the volume ratio of the n-hexane and ethyl acetate is 20:80; prepare the reverse phase with methanol and water To the mobile phase, as the reverse phase eluent of the sample, the volume ratio of the methanol and water is 40:60;

[0056] (2) Dissolution and filtration: Dissolve 500g of crude epothilone with a purity greater than 60% in n-hexane solution, filter it with a 0.45μm organic filter membrane after ultrasonication, and further dilute the filtrate with the normal phase mobile phase prepared in step (1) to a concentration of 0.1g / ml sample;

[0057] (3) Packing of dynamic axial compression column: 18000g of 200-800 mesh polar silica gel filler and 4500g of 40-75um non-polar silica gel bonded C18 chroma...

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Abstract

The present invention relates to the field of biochemistry, and discloses a method for separation purification of epothilone by using a dynamic axial compression column. The method comprises the following steps: mobile phase preparation, dissolution filtration, dynamic axial compression column filling, system balancing, normal phase separation purification and reverse phase elution separation. According to the present invention, purity of the prepared epothilone is more than 98.8%, and a yield is more than 98%; the process is simple, and the used organic solvents have characteristics of low price, low consumption and capability of recycling so as to effectively reduce production cost; an ultraviolet detector is adopted to perform online monitoring, operation is simple, efficiency is high, and product quality is easy to control; and isocratic elution is performed, performance requirements on equipment are low, a production cycle is short, a preparation time can be substantially saved with continuous sample injection, and efficient epothilone separation purification from the laboratory to the industry is achieved.

Description

technical field [0001] The invention relates to the field of biochemistry, in particular to a method for separating and purifying epothilone by using a dynamic axial compression column. Background technique [0002] Epothilones are a class of cytotoxic compounds secreted by Myxobacteria cellulosicum, with a 16-membered lactone macrocycle as the center body and thiazole ring ligand as the side chain. A new anti-tumor drug for tubulin polymerization and microtubule stabilization, CAS number: 152044-54-7, molecular formula: C27H41NO6S, molecular weight: 507.68, the main components are epothilone A and B, and they are 2: produced at a ratio of 1, are considered to be a novel class of naturally occurring inhibitors of microtubule depolymerization. [0003] Several epothilones have entered clinical trials: BMS-310750, another semi-synthetic analogue of epothilone B from Squibb; Epothilone B (EPO906) and its analogue (ABJ879); also Roche's epothilone D (KOS-862) and epothilone D ...

Claims

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Application Information

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IPC IPC(8): C07D493/04
Inventor 孟强孙娟戴士俊张俊张云海范金豹沈红艳周亮亮
Owner 江苏迪沃特仪器设备科技有限公司