A method for extracting 10-deacetylbaccatin III from southern yew

A southern yew, deacetylation technology, applied in the direction of organic chemistry and the like, can solve the problems of high production cost, complicated operation, long production time, etc., and achieve the effects of good effect, improved separation efficiency, and improved extraction rate.

Active Publication Date: 2021-06-11
无锡紫杉药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The domestic patent with the application number CN201510603454.2 discloses a method for preparing high-purity 10-deacetylbaccatin III from the branches and leaves of Taxus mandia as raw materials. The process steps are: rough extraction, sedimentation, adsorption, dissolution, Crystallization and recrystallization; this method dissolves the crude product through macroporous resin adsorption and different single solvents, removes a large number of insoluble impurities, and finally obtains high-purity 10-deacetylbaccatin III through repeated crystallization. But its operation is more complicated, the production time is long, and the production cost is higher

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] A method for extracting 10-deacetylbaccatin III from southern yew, comprising the following steps:

[0035] (1) After drying the southern yew branches and leaves, crush them through 30 sieves to obtain yew powder; immerse the yew powder in liquid nitrogen for 4 minutes and 5 dipping times; then carry out ammonia blasting treatment, wherein The reaction pressure is 2.5MPa, the reaction time is 20min, the solid-liquid ratio of yew powder and liquid ammonia is 1:7g / mL; then decompression blasting is carried out;

[0036] (2) Add petroleum ether (boiling range: 60-90°C) to the material obtained from step (1), the mass volume ratio of yew powder and petroleum ether is 1:5g / mL; ultrasonically extract at 35°C (Under normal pressure) 12min, the power during ultrasonic extraction is 100W; Filtrate, obtain filtrate;

[0037] (3) Adding ethanol with a mass concentration of 65% to the filtrate, the mass volume ratio of yew powder and ethanol is 1:13g / mL; extract at a constant temp...

Embodiment 2

[0043] A method for extracting 10-deacetylbaccatin III from southern yew, comprising the following steps:

[0044] (1) After drying the branches and leaves of the southern yew, crush them through 40 sieves to obtain yew powder; immerse the yew powder in liquid nitrogen, the immersion time is 3min, and the number of times of immersion is 3 times; then carry out ammonia blasting treatment, wherein The reaction pressure is 2MPa, the reaction time is 20min, the solid-liquid ratio of yew powder and liquid ammonia is 1:6g / mL; then decompression blasting is carried out;

[0045] (2) Add petroleum ether (boiling range: 60-90°C) to the material obtained from step (1), the mass volume ratio of yew powder and petroleum ether is 1:6g / mL; ultrasonically extract at 30°C 13min, the power during ultrasonic extraction is 100W; filter to obtain filtrate;

[0046] (3) Adding ethanol with a mass concentration of 65% to the filtrate, the mass volume ratio of yew powder and ethanol is 1:12g / mL; ex...

Embodiment 3

[0052] A method for extracting 10-deacetylbaccatin III from southern yew, comprising the following steps:

[0053] (1) After drying the southern yew branches and leaves, crush them through 30 sieves to obtain yew powder; immerse the yew powder in liquid nitrogen for 4 minutes and 5 dipping times; then carry out ammonia blasting treatment, wherein The reaction pressure is 2.5MPa, the reaction time is 25min, the solid-liquid ratio of yew powder and liquid ammonia is 1:8g / mL; then decompression blasting is carried out;

[0054] (2) Add petroleum ether (boiling range: 60-90°C) to the material obtained from step (1), the mass volume ratio of yew powder to petroleum ether is 1:7g / mL; ultrasonically extract at 35°C 15min, the power during ultrasonic extraction is 120W; filter to obtain filtrate;

[0055] (3) Add ethanol with a mass concentration of 65% to the filtrate, the mass volume ratio of yew powder and ethanol is 1:12g / mL; extract at a constant temperature at 52°C for 3h, and ...

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Abstract

The invention discloses a method for extracting 10-deacetylbaccatin III from Taxus chinensis, and relates to the technical field of natural product extraction. The method comprises the following steps: (1) crushing; liquid nitrogen treatment; ammonia blasting treatment (2) Petroleum ether ultrasonic removal of impurities; (3) Ethanol high-pressure constant temperature extraction; Ethanol ultrasonic extraction; (4) Concentration under reduced pressure, dissolved in acetone, filtration, and concentration to obtain crude extract one; (5) Upper macroporous adsorption resin , followed by washing with alkaline solution and deionized water, and then eluting with ethanol, collecting the eluent, concentrating to obtain crude extract II; (6) primary recrystallization: recrystallization with acetonitrile; (7) secondary recrystallization Crystallization: Acetone / petroleum ether system is used for recrystallization; the present invention has strong operability, rationally sets each step and strictly controls operating parameters, and can obtain 10-deacetylbaccatin III with excellent purity and yield, with a purity reaching More than 99.3%, the yield is more than 0.0242%.

Description

technical field [0001] The invention relates to the technical field of natural product extraction, in particular to a method for extracting 10-deacetylbaccatin III from Taxus chinensis. Background technique [0002] Southern yew (Taxus chinensis var.mairei) is a variety of Taxus (Taxaceae) in China, and it is a national first-class protected tree species. Paclitaxel in the yew plant belongs to diterpenoids and is currently the most effective anticancer drug. It is mainly used to treat ovarian cancer, breast cancer, lung cancer, colorectal cancer, melanoma, head and neck cancer, lymphoma, brain tumor It also has certain curative effect. 10-deacetylbaccatin Ⅲ (10-DABⅢ), the most important precursor of taxol in the biosynthesis of taxus plants, is also a diterpenoid taxane derivative, and is currently the semi-synthetic production of paclitaxel or docetaxel (polyene It is the main raw material of docetaxe). [0003] 10-Deacetylbaccatin III is mainly distributed in the branch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D305/14
CPCC07D305/14
Inventor 葛月兰高杰
Owner 无锡紫杉药业股份有限公司
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