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Extraction and purification method of 10-deacetylbaccatin III

A purification method and deacetylation technology are applied in the field of extracting and purifying 10-deacetyl baccatine III from the branches and leaves of Taxus chinensis, and can solve the problems of long time consumption, increased product cost, low production efficiency and the like

Pending Publication Date: 2021-04-23
CHONGQING ZHENYUAN HONGDOUSHAN DEV CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The deficiencies of the existing 10-deacetylbaccatin III industrialized production mainly include that in the purification process, most of the processes adopt silica gel chromatography separation and resin adsorption separation, and these two production processes take a long time, The production efficiency is low, leading to an increase in product costs, which squeezes out the company's due profits

Method used

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Examples

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Effect test

Embodiment 1

[0029] Weigh 100kg of southern yew branches and leaves (10-deacetylbaccatin III content 0.327%), dry it to a water content of ≤15%, crush it to a particle size of 10-20 mesh, add 80% methanol-water solution at 55°C Thermal cycle extraction 3 times:

[0030] For the first extraction, add 500L methanol-water mixed solvent and extract for 8 hours;

[0031] For the second extraction, add 300L methanol-water mixed solvent and extract for 8 hours;

[0032] For the third extraction, add 200L of methanol-water mixed solvent and extract for 4 hours;

[0033] Release the extract from the bottom of the extraction tank, combine the extracts three times to obtain about 820L of extract, concentrate to about 50L (weight 51.7kg) at 60°C and a vacuum of -0.060~-0.085MPa, add dichloromethane to the concentrate Extract 2 times:

[0034] Add 100L dichloromethane for the first extraction;

[0035] Add 50L dichloromethane for the second extraction;

[0036] About 160L of the obtained extracts ...

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PUM

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Abstract

The invention discloses an extraction and purification method of 10-deacetylbaccatin III, which comprises the following steps of treating taxus chinensis branches and leaves, extracting, filtering, concentrating, extracting, washing and concentrating to obtain a crude product A, carrying out freeze suction filtration on the crude product A to obtain a crude product B, and concentrating, freezing, filtering and washing the crude product B to obtain a crude product C, concentrating, freezing and filtering the crude product C to obtain a final extracted and purified 10-deacetylbaccatin III product. After taxus chinensis branches and leaves are extracted, a sodium bicarbonate aqueous solution is used for washing to remove acidic impurities and pigments in the material, so that the content of 10-deacetylbaccatin III in the extract concentrate is greater than or equal to 10%, the standard of acetonitrile washing can be achieved, a chromatographic separation step is omitted in the whole process, the production efficiency is improved, the production time is shortened, and after the crude product B is crystallized, the crude product B is washed with an acetone-n-hexane mixed solvent to remove pigment in the crude product B crystal. The content of the finally obtained 10-deacetylbaccatin III is as high as 99.23%, the purity reaches 99.37%, and the product yield reaches 75.99%.

Description

technical field [0001] The invention relates to the technical field of compound separation and purification, in particular to a method for extracting and purifying 10-deacetylbaccatin III from branches and leaves of Taxus chinensis. Background technique [0002] Paclitaxel and docetaxel are currently important taxane anticancer drugs, which are used for the treatment of advanced or metastatic breast cancer that failed prior chemotherapy, advanced or metastatic non-small cell lung cancer that failed cisplatin-based chemotherapy, combined with a Cyclophosphamide is used for the treatment of operable, node-positive breast cancer, combined with cisplatin for the first-line treatment of locally advanced or metastatic non-small cell lung cancer, combined with prednisone for the treatment of androgen-independent metastatic prostate cancer, combined with cisplatin Platinum and 5-fluorouracil first-line treatment of advanced gastric cancer. Paclitaxel naturally exists in Taxus chine...

Claims

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Application Information

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IPC IPC(8): C07D305/14
CPCC07D305/14
Inventor 徐胜博
Owner CHONGQING ZHENYUAN HONGDOUSHAN DEV CO LTD
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