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Separation and purification method of vinorelbine

A technology of vinorelbine and purification method, which is applied in the field of chemical pharmacy and separation and purification, can solve the problems of high cost and low separation efficiency, and achieve the effects of low production cost, high separation efficiency, and fast and simple operation process

Inactive Publication Date: 2008-10-15
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a method for separating and purifying vinorelbine, which solves the problems of high cost and low separation efficiency in existing methods, and is used for refining vinorelbine on a large scale

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Take 40g of grade III activated silica gel with a particle size of 50 μm, add 4g of diatomite (the mass percentage of diatomite and silica gel is 10%), add an equal volume of n-hexane and stir to form a suspension, pour A hollow PVC column with a diameter of 2.6cm is inserted into the plug with glass wool and a two-way piston. The silica gel-based filler is continuously deposited, and the solvent flows out through the glass wool. Transfer to PVC column, column height 13cm (column height-diameter ratio is 5: 1); Get 0.5g synthetic vinorelbine crude product (vinorelbine purity 25%, HPLC detection), the mass ratio of vinorelbine crude product to silica gel 1 / 80, dissolve the sample with 0.5mL methanol, under normal pressure, use methanol: n-hexane = 90:10 (V / V) solvent as the developing solvent, develop downward until the solvent reaches the bottom of the column, stop developing layer; the R of vinorelbine obtained with reference to the thin-layer experiment f value, ...

Embodiment 2

[0031](1) Take 80g of grade II activated silica gel with a particle size of 30 μm, add 16g of diatomite (the mass percentage of diatomite and silica gel is 20%), add an equal volume of petroleum ether and stir to form a suspension, pour A hollow PVC column with a diameter of 2.0cm is inserted into the plug with glass wool and a two-way piston. The silica gel-based filler is continuously deposited, and the solvent flows out through the glass wool. Transfer to PVC column, column height 40cm (column height-to-diameter ratio is 20: 1); Get 0.5g synthetic vinorelbine crude product (vinorelbine purity 27%, HPLC detection), the mass ratio of vinorelbine crude product to silica gel For 1 / 160, use 0.5mL methanol to dissolve the sample, under normal pressure, use methanol:dichloromethane=95:5 (V / V) solvent as the developing solvent, develop downward until the solvent reaches the bottom of the column, stop Exhibit layer; The R of vinorelbine obtained with reference to the thin-layer expe...

Embodiment 3

[0035] (1) Take 400g of grade III activated silica gel with a particle size of 80 μm, add 40g of diatomite (the mass percentage of diatomite and silica gel is 10%), add an equal volume of petroleum ether and stir to form a suspension, pour A hollow PVC column with a diameter of 4.3cm is inserted into the plug with glass wool and a two-way piston. The silica gel-based filler is continuously deposited, and the solvent flows out through the glass wool. The outflow speed of the solvent is controlled so that the surface of the silica gel-based filler is always covered by the solvent until the filler is completely Transfer to PVC column, column height 43cm (column height-diameter ratio is 10: 1); Get the vinorelbine crude product (vinorelbine purity 28% that HPLC detects) that 5.0g synthetically obtains, the mass ratio of vinorelbine crude product to silica gel 1 / 80, dissolve the sample with 1.0mL methanol, under normal pressure, use methanol: n-hexane = 98:2 (V / V) solvent as the dev...

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Abstract

A separation and purification method of vinorelbine belongs to the chemical pharmacy and separation and purification method, solving the problems of the prior method including high cost and low separation efficiency and used in the large-scale manufacturing of refined vinorelbine. The invention comprises the following: (1) a step of separating silica gel dry column, during which, chemically semisynthetic vinorelbine crude product is loaded on the silica gel dry column through wet method and is outspread downwards by means of developing solvent and pressure difference under ordinary pressure so as to obtain vinorelbine dry column chromatogram moderately separated product; (2) a step of reversed phase chromatography refining, during which, the medium-pressure and low-pressure reversed phase chromatography of the moderately separated product is carried out through adopting C18 filler as stationary phase and the mixed solution of methanol and water as mobile phase; (3) a step of crystallization, during which, the vacuum distillation of positive composition obtained through reversed phase chromatography is carried out, and then methanol is added to obtain 98.5 percent of refined vinorelbine. The invention has simple operation, less dosage of solvent, low production cost, high separation efficiency and high recovery rate; moreover, the purity of the made vinorelbine is above 98.5 percent and separation overall recovery rate is above 60 percent; therefore, the vinorelbine is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to chemical pharmacy and a separation and purification method, in particular to a separation and purification method of vinorelbine. Background technique [0002] Vinorelbine (Vinorelbine, Naveibine, VRL), also known as norvinblastine, isovinblastine, decarbavinblastine or demethyl dehydrovinblastine, was first synthesized by French scholar Potier in 1974. At present, vinblastine extracted from periwinkle or vindolin and vinblastine can be used as raw materials and obtained through chemical semi-synthesis. Vinorelbine has high anti-cancer activity and broad anti-tumor spectrum. According to foreign clinical studies, it has shown outstanding curative effect in the treatment of non-small cell lung cancer, breast cancer, ovarian cancer, malignant lymphoma, etc. with single drug or combined drug. [0003] Xia Desheng published in publication number CN1552715 in 2003, titled "preparation method of vinorelbine synthetic intermediate de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D519/04
Inventor 赵春芳余龙江李硕吴泽强熊茵
Owner HUAZHONG UNIV OF SCI & TECH
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