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Coarse taxol product separating and purifying process

A technology for separation and purification of paclitaxel, applied in the field of separation and purification of plant extracts, to achieve the effects of safe operation, large sample loading and high yield

Inactive Publication Date: 2004-09-08
丁志坚
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The disadvantage of the existing separation and purification method is that the primary yield of paclitaxel (that is, from the beginning of feeding, through the sequential technological process, and the yield of the output obtained is calculated as the active ingredient paclitaxel

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] ① 100 grams of paclitaxel crude product with a paclitaxel content of 15.6% in the raw material sample, wherein the paclitaxel net content is 15.6 grams;

[0027] ② Paclitaxel sample raw materials were dissolved in 300 ml of 95% (V / V) polar solvent ethanol, then water was added until the ethanol concentration was 60% (V / V), and the weight ratio of sample to ethanol aqueous solution was about 1:5;

[0028] ③ 1000 grams of macroporous adsorption resin AB-8, the weight ratio of which to the sample is 10 to 1, put it into a glass chromatography column with an outer diameter of 6 cm and a filling height of 100 cm;

[0029] ④ Load the sample from the top of the chromatographic column of the macroporous adsorption resin, that is, pour the sample solution into the chromatographic column, adjust the outlet valve of the chromatographic column, and control the flow rate of the solution in the chromatographic column to 1 liter / hour;

[0030] ⑤ Collect the effluent after chromatograp...

Embodiment 2

[0037] Use macroporous adsorption resin D101, ①~⑥ step other conditions are identical with embodiment 1;

[0038] ⑦5~20 parts of effluent are part II, wherein the content of paclitaxel is less than that of cephalomannine, concentrated and dried to obtain 8.55 grams of paclitaxel intermediate product A, which contains 38.5% of paclitaxel, that is, the net content of paclitaxel is 3.29 grams, accounting for 3.29 grams of paclitaxel in raw materials 21.09% of Paclitaxel;

[0039] ⑧The effluent from 21~termination is the third part, wherein the paclitaxel content is greater than the cephalomannine content, concentrated and dried to obtain 17.5 grams of paclitaxel intermediate product B, which contains 53.5% of paclitaxel, that is, the paclitaxel net content is 9.36 grams, accounting for paclitaxel in the raw material 60.01% of.

[0040] The net content of paclitaxel in the paclitaxel intermediate products A and B is 12.65 grams altogether, accounting for 81.1% of the paclitaxel i...

Embodiment 3

[0043] Use macroporous adsorption resin D201, ①~⑥ step other conditions are identical with embodiment 1;

[0044] ⑦5~20 parts of effluent are part II, wherein paclitaxel content is less than cephalomannine content, concentrated and dried to obtain paclitaxel intermediate product A8.765 grams, wherein containing paclitaxel 40.2%, that is, paclitaxel net content is 3.52 grams, accounting for 3.52 grams of paclitaxel in raw materials 22.57% of Paclitaxel;

[0045] ⑧The effluent from 21~termination is part III, wherein the paclitaxel content is greater than the cephalomannine content, concentrated and dried to obtain 18.5 grams of paclitaxel intermediate product B, which contains 50.2% of paclitaxel, that is, the paclitaxel net content is 9.19 grams, accounting for paclitaxel in the raw material 59.53%.

[0046] The net content of paclitaxel in the paclitaxel intermediate products A and B is 12.81 grams altogether, accounting for 82.1% of the paclitaxel in the raw material, that ...

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PUM

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Abstract

The present invention separates and purifies taxol by means of column chromatographic process with macroporous resin, such as AB-8, D101, D201 and AK-9 as fixed phase and polar solvent, such as water solution of ethanol or acetone, as flowing phase, with the effluent flow rate is 0.6-1.5 L / hr. The effluent with taxol content lower than cephalotmannine content is concentrated and dried to obtain intermediate taxol product A; and effluent with taxol content higher than cephalotmannine content is concentrated and dried to obtain intermediate taxol product B. The said process can separate and purify coarse taxol product with 9-20% content to obtain intermediate taxol product with 40-60% content in the yield as high as 80%. The process can eliminate water soluble impurity from the coarse product.

Description

(1) Technical field [0001] The invention relates to the field of separation and purification of plant extracts, in particular to a method for separating and purifying paclitaxel from crude paclitaxel products. (2) Technical background [0002] Paclitaxel is the most promising anticancer drug discovered in the world in the past two decades. It has good curative effect on the treatment of breast cancer, ovarian cancer, esophageal cancer, lung cancer, liver cancer and other cancers, and has a strong lethality to cancer cells. Toxic and side effects are minimal. Therefore, it has become the focus of current pharmaceutical industry research. [0003] Paclitaxel belongs to the group of diterpene alkaloids. At first, paclitaxel was extracted and isolated from the natural plant yew. Taxus is a rare species. Natural yew resources are extremely limited, and yew grows slowly. Natural yew cannot meet the demand for paclitaxel production. In order to open up a new source of paclitaxe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/14
Inventor 丁志坚徐位坤
Owner 丁志坚
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