Method for extracting 10-deacetylbaccatin III from taxus chinensis

A technology for deacetylation and yew, applied in the field of extracting 10-deacetyl baccatine III from yew, can solve the problems of large influence, large cost input, obvious effect and the like, and achieves reduction of production cost and low production cost , the effect of high extraction yield

Active Publication Date: 2018-04-06
上海卓鼎生物技术有限公司
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  • Abstract
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Problems solved by technology

[0009] (1) At present, most methods for extracting 10-desacetylbaccatin III use solvents such as methanol, ethanol or methanol water, ethanol water as extraction solvents; due to the polar nature of these solvents, various impurities in Taxus chinensis It is extracted together with 10-deacetylbaccatin III, which increases the difficulty of subsequent column chromatography, and the impurities cannot be effectively controlled; the product quality is reduced and the extraction cost is increased;
[0010] (2) According to the extraction methods in most literature patent reports, more than 90% of the impurities in the obtained methanol or ethanol paste are useless during the extraction process and need to be removed. During industrial production, it increases the difficulty of industrial production. Some use alcohol The method of sinking to remove impurities, the effect is obvious but affects the yield; some add sodium bicarbonate or weak alkaline solution to extract during extraction, which can also achieve the effect of removing impurities, but the introduction of alkali, alkali on 10-deacetyl The impact of baccatin III is relatively large, and many degradation impurities caused by weak bases are often derived during the production process; this seriously affects the quality of 10-deacetylbaccatin III and the control of production costs;
[0011] (3) Due to the use of a large amount of methanol or ethanol in the subsequent processing of the substances extracted by the traditional process, various pigments, gums, and tannins are discharged together with water, which seriously affects the water body and the environment; industrial production The investment in the environment increases the processing cost of the enterprise from another angle;
[0012] (4) The traditional extraction process requires complicated column chromatography production, which has a long production period and high cost investment

Method used

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  • Method for extracting 10-deacetylbaccatin III from taxus chinensis

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Experimental program
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Embodiment 1

[0032] Embodiment 1: This industrialized method for extracting 10-DAB from the branches and leaves of Taxus chinensis, the specific operations are as follows:

[0033] (1) Add 1 kg of dried Yunnan yew branches and leaves with a 10-DAB content of about 4‰ in a 10L pot, add 5L of pure tap water, and drop 2.5 mL of glacial acetic acid at the same time, mix well and soak at 45-50°C for 4 hours , filter, soak the filter residue with an aqueous solution containing a stabilizer (volume concentration of 0.5‰ glacial acetic acid solution), soak twice, and combine the soaking solution; use 4L ethyl acetate to extract the soaking solution, keep stirring for 1 hour, and let it stand for separation layer, the ethyl acetate layer was taken out, the remaining liquid was extracted twice with ethyl acetate again, the three extracts were combined, and then concentrated and dried under reduced pressure at 60°C to obtain 25.86 g of a light yellow-green solid, which was tested for the content of 10...

Embodiment 2

[0036] Embodiment 2: This industrialized method for extracting 10-DAB from the branches and leaves of Taxus chinensis, the specific operations are as follows:

[0037] (1) Add 10kg of dried Yunnan yew branches and leaves with a 10-DAB content of about 4‰ in a 50L pot, add 60L of pure tap water, and drop 48mL of glacial acetic acid at the same time, mix well and soak at 40-45°C for 5 hours, Filter, soak the filter residue with an aqueous solution containing a stabilizer (volume concentration of 0.8‰ glacial acetic acid aqueous solution), soak repeatedly 3 times, and combine the soaking solution; use 35L ethyl acetate to extract the soaking solution, keep stirring for 0.8h, and let stand to separate layer, the ethyl acetate layer was taken out, the remaining liquid was extracted 3 times again, the 4 extracts were combined, and then concentrated and dried under reduced pressure at 65°C to obtain 300.1 g of a light yellow-green solid, which was detected to have a 10-DAB content of ...

Embodiment 3

[0040] Embodiment 3: This industrialized method for extracting 10-DAB from the branches and leaves of Taxus chinensis, the specific operations are as follows:

[0041] (1) Add 1 kg of dried Yunnan yew branches and leaves with a 10-DAB content of about 4‰ in a 10L pot, add 7L of pure tap water, and drop 7 mL of citric acid at the same time, mix well and soak at 45-50°C for 3 hours , filter, soak the filter residue with an aqueous solution containing a stabilizer (citric acid volume concentration is 1‰), soak twice, and combine the soaking solution; use 6L ethyl acetate to extract the soaking solution, keep stirring for 0.5h, and let stand to separate layer, the ethyl acetate layer was taken out, the remaining liquid was extracted 3 times again, the 4 extracts were combined, and then concentrated and dried under reduced pressure at 70°C to obtain 26.3 g of a light yellow-green solid, which was detected to have a 10-DAB content of 14.5%. The rate is about 95%;

[0042] (2) Disso...

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Abstract

The invention discloses a method for extracting 10-deacetylbaccatin III from taxus chinensis. The method comprises the following steps: soaking and extracting 10-deacetylbaccatin III in taxus chinensis by adopting an aqueous solution containing a stability maintainer; and extracting, performing discoloring and flocculating treatment, recrystallizing and the like, thereby obtaining the high-purity10-deacetylbaccatin III. The method disclosed by the invention is clean, low in cost, non-harsh in extraction conditions, less in by-products, less in pigments and high in extraction rate, and is applicable to industrialized production and market popularization and application.

Description

technical field [0001] The invention relates to an industrial production method for extracting 10-deacetylbaccatin III from branches and leaves of Taxus yunnanensis. Background technique [0002] 10-Deacetylbaccatin III is a natural taxane contained in Taxus chinensis, which is the starting material or intermediate for the production of docetaxel, semi-synthetic paclitaxel, and cabazitaxel. [0003] 10-Deacetylbaccatin III, CAS NO: 32981-86-5, the structural formula is as follows: [0004] [0005] According to statistics, there are about 76 million cancer patients in the world, with an increase of 10 million every year. In 2007, 7.6 million patients died of malignant tumors, accounting for 12% of the total number of deaths. In developed countries, the number of people who died of malignant tumors Accounted for 21.6% of the total number of deaths. In China, the incidence of malignant tumors is particularly rapid. At present, there are about 4.5 million cancer patients i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/14
CPCC07D305/14
Inventor 马回民杨青春胡倩马怀虎
Owner 上海卓鼎生物技术有限公司
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