Method for separating and purifying 10-deacetyl Baccatins III

A technology for removing acetylation and ethyl acetate, which is applied in the field of separation and purification of 10-deacetylbaccatin III combined with forward and reverse phase liquid chromatography technology, can solve the problems of incomplete separation of impurities, small processing capacity, and high cost, and achieve The solvent is easy to recycle and cheap, prolongs the service life, and has the effect of low cost

Active Publication Date: 2007-10-03
北京信汇科技有限公司
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Problems solved by technology

[0015] The above-mentioned method mainly adopts alcohol solvent to extract 10-DABIII in the branches and leaves of Taxus chinensis, and then respectively adopts methods such as crystallization, normal phase silica gel column chromatography or reversed phase chromatography to carry out purification, therefore, these methods have the following defects: the yield is low , Incomplete separation of impurities, small processing capacity, and large use of organic solvents lead to high costs

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  • Method for separating and purifying 10-deacetyl Baccatins III
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  • Method for separating and purifying 10-deacetyl Baccatins III

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Embodiment 1

[0037] Refer to Figure 1 for the process flow diagram of this embodiment, and refer to Figure 2 for the serial connection of the pretreatment column and the separation column.

[0038] (1) Take 1 kg of pulverized European yew (T.baccata) branches and leaves, add 7L of 50% methanol aqueous solution, keep a constant temperature water bath at 40°C, stir and extract for 8 hours, filter to obtain a primary extract and a primary filter residue;

[0039] (2) Return the primary filter residue to the extraction container, then add 5L of 50% methanol aqueous solution, keep a constant temperature water bath at 40°C, stir and extract for 8 hours, and filter to obtain the secondary extract and secondary filter residue;

[0040] (3) return the secondary filter residue to the extraction container, then add 5L of 50% methanol aqueous solution, keep a constant temperature water bath at 40° C., stir and extract for 8 hours, and filter to obtain three extractions and three filter residues;

[00...

Embodiment 2

[0055] Get 1 kilogram of Canadian yew (T.canadensis), and the specific operation steps are the same as in Example 1, and the difference is: the extract in step (1) is replaced with 70% acetone, and leached three times; the fixation in step (10) The phase is replaced by coated polystyrene-divinylbenzene, the eluent in step (11) is replaced by 5-50% ethanol aqueous solution, and the separation is repeated twice; the extractant in step (13) is replaced by butyl acetate , the crystallization agent in the step (14) was replaced with petroleum ether; after drying, 0.23 g of 10-DABIII with a purity of 99.61% was obtained, and the yield was 78%.

Embodiment 3

[0057] Get 1 kilogram of Yunnan yew (T.yunnanensis), and the specific operation steps are the same as in Example 1, and the difference is that the extract in step (1) is replaced with 65% ethanol, and leached three times; the fixation in step (10) The phase is replaced by cross-linked polystyrene-divinylbenzene, the eluent in step (11) is replaced by 5-50% acetonitrile aqueous solution, and the separation is repeated twice; the extractant in step (13) is replaced by methyl acetate , the crystallization agent in step (14) was replaced by cyclohexane; after drying, 0.18 g of 10-DABIII with a purity of 99.55% was obtained, and the yield was 76%.

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Abstract

This invention relates to a kind of separation and purification method of 10- DABIII. This invention adopts positive and negative phase chromatographic technique combinding, takes normal phase color spectrum as first order hand ling, remove most impurity, in favor of protecting high cost reversion phase chromatography support, prolong its service life; whereas reversion phase chromatography could hand larger sample quantity, and has better removal effect to the impurity that normal phase colour spectrum unease separate off, solvent is easy reclaim and cost is cheaper. So the combinding of positive and negative phase chromatographic technique not only could obtain 10 -DABIII, but also be able to reduce cost. Besides, this invention also adopts two-stage color spectrum tand em isolation techniques, through pretreatment post to separate a part of impurity, then cascaded separating column to carry out subdivision, advance separating effect, increase load sample quantity of chromatographic column.

Description

technical field [0001] The invention relates to a method for separating and purifying 10-deacetylbaccatin III, in particular to a method for separating and purifying 10-deacetylbaccatin III in combination with forward and reverse phase liquid chromatography techniques. Background technique [0002] The molecular structural formula of 10-deacetylbaccatin III (10-Deacetylbaccatin III, hereinafter referred to as 10-DABIII) is as follows: [0003] [0004] 10-DABIII is the main raw material for the synthesis of anticancer drug docetaxel and semi-synthetic paclitaxel. It mainly exists in the branches, leaves, bark and roots of Taxus chinensis. With the confirmation of the unique curative effect of taxane-based anticancer drugs, the market demand for such drugs is increasing day by day, which urgently requires more economical and reasonable utilization of existing taxus plants, as much as possible and efficiently from Separation and purification of the substances required for ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/14
Inventor 朱德权张平苏萌
Owner 北京信汇科技有限公司
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