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Method for separating and purifying paclitaxel and cephalomannine

A technology of cephalomannine and paclitaxel, which is applied in the field of high-performance liquid phase preparative chromatographic separation, can solve problems such as complex processes, and achieve the effects of simple operation methods, low requirements for instruments, and good method stability

Inactive Publication Date: 2015-03-18
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the disadvantages of the prior art such as complicated process, and introduces a simple method for separating and purifying paclitaxel and cephalomannine

Method used

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  • Method for separating and purifying paclitaxel and cephalomannine

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Effect test

Embodiment 1

[0031] Chromatographic conditions: detection machine: Dianne Summit high performance liquid chromatography system;

[0032] Chromatographic column: MKF-EP-RP (300mm×7.8mm, 8μm); mobile phase: acetonitrile (B) / water (A) = 75:25 (volume ratio, the same as above); flow rate: 1mL / min; detection wavelength: 229nm; Injection volume: 20 μL; Injection substance: Test product-1, the measured resolution R of paclitaxel and cephalomannine is 0.84.

Embodiment 2

[0034] Chromatographic conditions: detection machine: Dianne Summit high performance liquid chromatography system;

[0035] Chromatographic column: MKF-EP-RP (200mm×8.0mm, 8μm); mobile phase: acetonitrile (B) / water (A) = 60:40 (volume ratio, the same as above); flow rate: 1mL / min; detection wavelength: 229nm; Injection volume: 20 μL; Injection substance: Test product-2, the measured resolution R of paclitaxel and cephalomannine is 1.04.

Embodiment 3

[0037] Chromatographic conditions: detection machine: Dianne Summit high performance liquid chromatography system;

[0038] Chromatographic column: MKF-EP-RP (600mm×7.8mm, 12μm); mobile phase: acetonitrile (B) / water (A) = 50:50 (volume ratio, the same as above); flow rate: 1.5mL / min; detection wavelength : 229nm; Injection volume: 20 μL; Injection substance: Test product-3, the measured resolution R of paclitaxel and cephalomannine is 1.27.

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Abstract

The invention relates to a method for separating and purifying paclitaxel and cephalomannine. According to the method disclosed by the invention, a preparative high performance liquid chromatography is adopted, and the chromatographic conditions are that a polystyrene-divinyl benzene copolymer chromatographic column refers to MKF-EP-RP with the diameter of 5-12 microns and the size of (150-600)*(7.0-20.0)mm (I.D.), a mobile phase comprises acetonitrile and water according to a volume ratio of (45-60) to (40-55), the flow velocity is equal to 1.0-3mL / min, the detection wavelength is equal to 229nm and the sample size is equal to 20-100 microL. According to the method disclosed by the invention, the defects such as irreversible adsorption of media such as silica gel and complicated process flow are overcome, and paclitaxel products with the purity of over 98 percent can be obtained by further separation.

Description

(1) Technical field [0001] The invention relates to a high-performance liquid phase preparative chromatography (HPLC) separation method, in particular to a preparation method for separating and purifying paclitaxel and cephalomannine with a polystyrene gel chromatography medium as a carrier. (2) Background technology [0002] Paclitaxel is a diterpenoid isolated from Taxus genus plants and has broad-spectrum anticancer activity. It has a unique anti-cancer mechanism and has good curative effect on the treatment of ovarian cancer, melanoma, lung cancer, breast cancer and other cancers. In recent years, it has become the hottest new drug in the field of natural plant medicine, and its demand is increasing day by day. Since paclitaxel is mainly derived from the bark of Taxus chinensis, the resources are scarce and the content is low, and the purity of paclitaxel is required in clinical applications, so it will be a huge and complicated project to separate and extract high-puri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 刘晓宁黄艳魏荣卿
Owner NANJING UNIV OF TECH
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