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Method for high efficiency separating and purifying 1-deacetyl Baccatins III (10-DABIII)

A technology of separation, purification and deacetylation, which is applied in the direction of organic chemistry, can solve problems such as yield loss, large solvent consumption, and reduced solvency, so as to improve the separation degree and separation peak shape, increase yield and purity, and demand Reduced effect

Inactive Publication Date: 2007-10-03
CHENGDU PUSH BIOLOGICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Chinese Patent Application No. 02136678 discloses a method for extracting 10-DABIII from ethanol-extracted yew branches and leaves residues, and adopts normal phase preparative chromatography to separate and obtain pure product 10-DAB III. Although mentioned in this separation and purification method Preparative liquid chromatography separation process, but the solvent system and gradient elution method used in large-scale production appear to be complicated, the separation efficiency cannot be really improved in actual production, and there are disadvantages such as large solvent consumption
Because 10-DAB III is extracted to a certain degree of purity, its solubility in conventional solvents is reduced. The use of ethyl acetate mentioned in this patent cannot actually dissolve the semi-finished product 10-DAB III very well, because it needs to be industrialized. Preparative liquid chromatography for separation must find a more suitable eluent system
[0005] In addition, Chinese Patent Publication No. CN1473821A discloses a method for extracting 10-DAB III. In this patent, conventional silica gel chromatography is used to separate and extract the semi-finished product 10-DAB III. This method is time-consuming and consumes a large amount of solvent. Because of the irreversible adsorption of conventional silica gel, the recycling rate of silica gel is low, and the waste discharge is large, which is also easy to cause the loss of yield.

Method used

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  • Method for high efficiency separating and purifying 1-deacetyl Baccatins III (10-DABIII)
  • Method for high efficiency separating and purifying 1-deacetyl Baccatins III (10-DABIII)
  • Method for high efficiency separating and purifying 1-deacetyl Baccatins III (10-DABIII)

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Embodiment 1

[0031] Embodiment 1, the raw material of semi-finished product 10-deacetylbaccatin III is low content, and the method for sample dissolution and separation and purification has tetrahydrofuran

[0032] Take by weighing 100 grams of 10-DAB III raw material powder with a content of 23%, prepare a chromatographic column with a dynamic axial compression liquid phase of 100mm, the packing is spherical silica gel of 20-45um, and the aperture is 70A, and a total of 1650 grams of packing ( 10-DABIII: the weight ratio of packing is about 1.40%), the separation chromatographic column is 40cm long, and the mobile phase is 22:77:1=tetrahydrofuran:n-hexane:methanol (volume ratio).

[0033] Weigh 100 grams of 10-DAB III raw material powder with a content of 23%, use tetrahydrofuran at 50° C. to promote dissolution by ultrasonic waves, filter, and inject 50 grams of samples into the compressed liquid phase preparative chromatographic column each time. A mixed solution of tetrahydrofuran, n-h...

Embodiment 2

[0035] Example 2, the raw material of semi-finished product 10-deacetylbaccatin III has a high content, and the method for sample dissolution and separation and purification has tetrahydrofuran

[0036] Weigh 60 grams of 10-DAB III powder (content is 53%) of the raw material, prepare a chromatographic column with a dynamic axial compression liquid phase of 100mm, the packing is spherical silica gel of 20-45um, the aperture is 70A, and a total of 1650 grams are filled Packing (10-DAB III: the weight ratio of packing is about 1.92%), the length of separation chromatographic column is 35cm, and the mobile phase is 26:73:1=tetrahydrofuran:n-hexane:methanol (volume ratio).

[0037] Weigh 60 grams of 10-DAB III raw material powder with a content of 53%, promote dissolution with tetrahydrofuran at 55° C. by ultrasonic waves, filter, and inject 30 grams each time. A mixed solution of tetrahydrofuran, n-hexane and methanol is used as the mobile phase, and the separation time is 55 minu...

Embodiment 3

[0040] This embodiment is the same as the steps of embodiment 2, only THF:n-hexane:methanol (volume ratio)=30:68:2.

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Abstract

This invention relates to a high efficiency method of separation and purification 10 - DAB III. It utilizes tetrahydrofuran to dissolve semi-manufactured 10-DBA III, then add it to dynamic axial compression liquid phase preparative chromatographic column, adopts blend solvent of tetrahydrofuran, normal hexane and methanol as elution mobile phase, through one to twice separation, then be able to obtain 10 - DAB III of purity reaching 99 percent.

Description

technical field [0001] The present invention belongs to the technology of extracting medicinal substances from Taxus chinensis, especially the separation and purification of the semi-finished product 10-deacetylbaccatin III (interpreted as: 10-DAB III) extracted from Taxus chinensis into a high-purity fine product Methods. Background technique [0002] 10-Deacetylbaccatin III (10-DAB III), as a structural monomer mainly present in Taxus species, can be used as the precursor of semi-synthetic antineoplastic drugs paclitaxel and docetaxel. Paclitaxel and docetaxel have been clinically used in the treatment of breast cancer, ovarian cancer, lung cancer, etc., with good curative effect and low side effects, and have gradually become the first-line anti-tumor drugs. As the number of cancer patients increases year by year, the demand for paclitaxel and docetaxel is increasing day by day, and the demand for their raw materials is even greater. In the...

Claims

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Application Information

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IPC IPC(8): C07D305/14
Inventor 张黎刘丁董维珍
Owner CHENGDU PUSH BIOLOGICAL TECH
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