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Method for extracting 10-deacetyl baccatin III from Taxus chinensis var.mairei

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

Active Publication Date: 2019-12-10
无锡紫杉药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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PUM

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Abstract

The invention discloses a method for extracting 10-deacetyl baccatin III from Taxus chinensis var.mairei, and relates to the technical field of natural product extraction. The method comprises the following steps: (1) crushing is conducted, liquid nitrogen treatment is conducted, and ammonia gas blasting treatment is conducted; (2) petroleum ether is subjected to ultrasonic impurity removal; (3) ethanol is subjected to high-pressure and constant-temperature extraction and ultrasonic extraction; (4) decompression concentration is conducted, dissolution is conducted though acetone, filtering andconcentration are conducted, and thus a crude extract I is obtained; (5) macroporous adsorption resin is washed though an alkali solution and deionized water in sequence and then eluted with the ethanol, eluent is collected and concentrated, and thus a crude extract II is obtained; (6) primary recrystallization is conducted, specifically, recrystallization is conducted through acetonitrile; and (7) secondary recrystallization is conducted, specifically, recrystallization is conducted through an acetone / petroleum ether system. The method is high in operability, the steps are reasonably set, operation parameters are strictly controlled, the 10-deacetyl baccatin III with the excellent purity and yield can be obtained, the purity reaches 99.3% or above, and the yield is 0.0242% or above.

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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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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