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A kind of preparation method of high-purity paclitaxel compound

A technology for paclitaxel and compounds, which is applied in the field of preparation of high-purity paclitaxel compounds, can solve the problems of large consumption of chromatographic fillers, high production cost, large workload and the like, and achieves the effects of peak shape resolution, simple operation and high recovery rate.

Active Publication Date: 2012-02-22
SHANGHAI TAUTO BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, the method for extracting paclitaxel compounds is adsorption column chromatography or partition column chromatography. However, this type of method consumes a large amount of chromatography packing materials, and needs frequent replacement, cleaning and activation of packing materials in the production process, which not only makes the production cost very high. High, and the workload is heavy, the yield is low

Method used

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  • A kind of preparation method of high-purity paclitaxel compound
  • A kind of preparation method of high-purity paclitaxel compound
  • A kind of preparation method of high-purity paclitaxel compound

Examples

Experimental program
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Effect test

Embodiment 1

[0027] A high-speed countercurrent chromatography system with a column volume of 300ml was used for separation (equipped with NS-1007 pump, 8823A-UV ultraviolet detector and Yokogawa3057 portable recorder). Select n-hexane-ethyl acetate-acetone-water as the solvent system, arrange the above-mentioned solvent components in a separatory funnel according to the volume ratio of 7:3:5:5, shake well, and then let stand to separate layers. After equilibrating for a period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase).

[0028] Weigh 200mg of paclitaxel crude extract, heat and dissolve with 20ml of stationary phase for later use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine, pump the mobile phase into the column until a dynamic balance is established, and inject samples through the injection valve; then receive the target components according to the detection spectrum. After the ta...

Embodiment 2

[0030] A high-speed countercurrent chromatography system with a column volume of 1000ml was used for separation. Petroleum ether-chloroform-methanol-water was selected as the solvent system, and the above solvent components were arranged in a separatory funnel according to the volume ratio of 3:7:3:5, shaken up and then allowed to stand for stratification. After equilibrating for a period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase).

[0031] Weigh 1g of paclitaxel crude extract, heat and dissolve with 50ml of stationary phase for later use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine, pump the mobile phase into the column until a dynamic balance is established, and inject samples through the injection valve; then receive the target components according to the detection spectrum. After the target fraction is evaporated to dryness, it can be crystallized with methanol to o...

Embodiment 3

[0033] A high-speed countercurrent chromatographic system with a column volume of 5000ml was used for separation. Petroleum ether-diethyl ether-ethanol-water was selected as the solvent system, and the above-mentioned solvent components were arranged in a separatory funnel according to the volume ratio of 70:70:30:70, and the mixture was left to stand and separate after shaking. After equilibrating for a period of time, separate the upper phase (stationary phase) and the lower phase (mobile phase).

[0034] Weigh 5g of paclitaxel crude extract, heat and dissolve with 250ml stationary phase for later use. Before sample injection, fill the entire column with stationary phase, adjust the speed of the main engine, pump the mobile phase into the column until a dynamic balance is established, and inject samples through the injection valve; then receive the target components according to the detection spectrum. After the target fraction is evaporated to dryness, it can be crystalliz...

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Abstract

The invention adopts high-speed countercurrent chromatography (HSCCC) to provide a preparation method of a high-purity paclitaxel compound. The method comprises steps: (1) pretreatment, 200mg-5g paclitaxel crude extract is heated and dissolved with 20ml-250ml stationary phase for use; , component D according to the volume ratio of 3-7:3-7:3-7:3-7, shake well and stand to separate the upper phase and the lower phase, the upper phase is used as a stationary phase, and the mobile phase is pumped into the column Inside, the sample is injected by the injection valve, and the target component is received according to the ultraviolet spectrum of the detector; (3) post-processing, the collected paclitaxel fraction is concentrated to dryness under reduced pressure to obtain a white solid, which is dissolved and crystallized, and obtained after filtration and drying. Needle-like crystals, the crystals are detected by HPLC, and the purity is above 99%. The method has high yield and low cost.

Description

technical field [0001] The invention relates to a preparation method of plant medicine, in particular to a preparation method of a high-purity paclitaxel compound. Background technique [0002] Paclitaxol is a new type of natural anti-cancer drug, which is extracted from Taxus chinensis. It has good anti-cancer activity and has obvious curative effect on various tumors. Its anti-cancer mechanism lies in promoting the polymerization of microtubules, forming Stable inactive microtubule polymers, thereby affecting the mitosis of tumor cells, resulting in cell death. In 1992, the U.S. Food and Drug Administration (FDA) approved paclitaxel for marketing. At present, it has been proved that paclitaxel has a very significant effect on breast cancer, ovarian cancer, head and neck cancer and non-small cell lung cancer, and has been gradually applied to these types of cancer. in treatment. [0003] The structural formula of paclitaxel is as follows: [0004] [0005] The molecul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/14
Inventor 符晓晖苏玉萍邓秋云
Owner SHANGHAI TAUTO BIOTECH CO LTD
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