Separation and purification method for vinca alkaloids

A separation and purification, alkaloid technology, applied in the direction of organic chemistry, can solve the problems of large solvent consumption, cumbersome operation, serious environmental pollution, etc., and achieve the effect of simple operation, good separation effect and high degree of automation

Active Publication Date: 2010-02-03
GUANGZHOU HANFANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Among the above-mentioned methods, not only are the technical specificity strong, but also generally require repeated column passing and multiple recrystallizations, cumbersome operation, large solvent consumption, and thus serious environmental pollution problems

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] The separation and purification of embodiment 1 vinblastine

[0019] Get vinblastine crude product (content 65%) 10g, dissolve with 20ml dichloromethane, apply the wet method of alumina column chromatography (200g aluminum oxide), elute with dichloromethane, thin-layer chromatography (TLC) detects and follows the column layer After analyzing the separation, the fractions containing vinblastine were collected and concentrated to dryness under reduced pressure at 30-35°C to obtain 8.5 g of vinblastine pretreated product.

[0020] Take 5 g of vinblastine pretreated product, add 10 ml of dichloromethane to dissolve, manually inject sample, dichloromethane-ethanol gradient elution, flow rate 40 ml / min. (Preparation of column packing: 200-300 mesh, 200 g of silica gel, column pressure: 80-100 bar). A UV detector was used to track the separation of the column chromatography, and TLC was used to collect and classify fractions. The main components rich in vinblastine were comb...

Embodiment 2

[0021] The separation and purification of embodiment 2 vincristine

[0022] Get vincristine crude product (content 63%) 5g, dissolve with 10ml dichloromethane, apply the wet method of aluminum oxide column chromatography (aluminum oxide 200g), elute with dichloromethane, TLC detects and tracks the separation situation of column chromatography, The fractions containing vincristine were collected and concentrated to dryness at 40-45°C under reduced pressure to obtain 8.3 g of vincristine pretreated product.

[0023] Take 5 g of vincristine pretreated product, add 10 ml of dichloromethane to dissolve, manually inject sample, dichloromethane-ethanol gradient elution, flow rate 50 ml / min. (Preparation of column packing: 200-300 mesh, 200 g of silica gel, column pressure: 80-100 bar). A UV detector was used to track the separation of the column chromatography, and TLC was used to collect and classify fractions. Merge the main components rich in vincristine, concentrate to dryness ...

Embodiment 3

[0024] The separation and purification of embodiment 3 vindesine

[0025] Take 5 g of vindesine crude product (content 65.0%, HPLC), add 10 ml of chloroform to dissolve, manually inject sample, chloroform-methanol gradient elution, flow rate 50 ml / min. (Preparation of column packing: 200-300 mesh, 200 g of silica gel, column pressure: 80-100 bar). The ultraviolet detector tracks the separation of the column layer, and is accompanied by TLC to collect and classify the fractions. The main components rich in vindesine were combined, concentrated to dryness at 35±10°C under reduced pressure to obtain 2.3 g of vindesine free base, with a content of 95.0% (HPLC), and recrystallized with methanol-ethanol to obtain 1.9 g of vindesine, with a content of 95.0%. 97.2% (HPLC).

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Abstract

A separation and purification method for vinca alkaloids comprises the following steps: (1) the pretreatment of coarse crude products: putting vinca alkaloids crude product on an aluminum oxide column, eluting and collecting alkaloid fraction, combining and then decompressing and concentrating till being dry to obtain a pretreated product; (2) high performance liquid chromatography separation: firstly preparing chromatographic column stationary phase, filling being silica gel, sample handling, gradient elution, following the situation of the preparative chromatography separation by a detector,thin layer chromatography or high efficient liquid phase detection, and combining enriched vinca alkaloids fraction; (3) recrystallization: decompressing and concentrating alkaloid fraction till being dry, dissolving lower alkyl alcohols, laying aside, crystallizing, filtering and drying. The method is suitable for the separation and purification of the vinca alkaloids, does not need particular filling, also does not need to use high toxicity solvent, is simple to operate, has high automatic degree, good separation effect; the filling used by stationary phase is packed into the column at onetime and used for many times. Mobile phase can be recycled, is environmental friendly, economic and suitable for industrialization production.

Description

technical field [0001] The invention relates to vinblastine alkaloids, in particular to a method for separating and purifying vinblastine alkaloids. Background technique [0002] Vinblastine is one of the alkaloids contained in Catharanthus roseus. As an antimitotic drug, it can inhibit microtubule polymerization and induce self-associated tubulin to form coiled helical complexes. In the past 50 years since vinblastine was isolated in 1958, a series of vinblastine derivatives including vinblastine have been chemically synthesized, including vinblastine, vincristine, vindesine, vinorelbine, etc. Vinblastine alkaloids have been used as a large class of important antineoplastic drugs today. [0003] Vinblastine extracted from plants or vinblastine alkaloids obtained by chemical semi-synthesis generally contain more impurities. In addition, due to the complex structure of vinblastine alkaloids, their properties are not stable, and they are easily deteriorated when exposed to h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D519/04
Inventor 黄翔冯锦玲陈日星张燕娜罗展良梁丽思
Owner GUANGZHOU HANFANG PHARMA
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