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Method for separating and purifying 10-deacetyl baccatin III from Chinese yew branches and leaves

A technology for deacetylation of yew branches and leaves, which is applied in the field of extraction of yew plant components, can solve the problems of low reuse rate and high cost, and achieve the effects of simplification of solvent types, reduction of emissions and treatment, and easy recycling

Active Publication Date: 2013-09-25
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

However, this method uses a large amount of organic solvent in the extraction process, and the normal phase chromatography uses silica gel as a stationary phase, which has a low recycling rate and high cost

Method used

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  • Method for separating and purifying 10-deacetyl baccatin III from Chinese yew branches and leaves
  • Method for separating and purifying 10-deacetyl baccatin III from Chinese yew branches and leaves
  • Method for separating and purifying 10-deacetyl baccatin III from Chinese yew branches and leaves

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] (1) Take 1 kg of crushed European yew branches and leaves (the content of branches and leaves is 1230ppm), put them into a glass column of 100mm×1000mm, add 0.5% by volume of acetic acid aqueous solution (temperature is 50°C) for diafiltration, and the leachate Combined and stirred evenly, a total of 15L, the effective amount of 10-DABⅢ detected by HPLC was about 1.2g.

[0054] (2) Adsorb leachate with D101 macroporous adsorption resin that has been treated and packed into a 100mm×500mm glass column (resin treatment method is to soak in methanol for 12 hours, and then rinse methanol with drinking water before use). Elute with ethyl acetate after all the adsorption, concentrate and dry the eluent (about 4.5L) to obtain a dry paste of about 35g, add 105ml of acetonitrile to the dry paste to dissolve the crystals at 70°C, let stand at 15°C for 4h, and pump Filter, and dry the filter cake to obtain 3.4 g of crude product, and the detected 10-DABⅢ content is 31.4%.

[0055]...

Embodiment 2

[0057] (1) Take 300kg of crushed European yew branches and leaves and pack them into 6m 3 In the diafiltration tank, add 2% acetic acid aqueous solution (temperature 40°C) for diafiltration, and mix the leachate in batches, with a total of about 5000m 3 , The effective amount of 10-DABⅢ detected by HPLC is about 356g.

[0058] (2) Put the D101 resin into a 600L stainless steel column after being treated according to the method in Example 1, and absorb the leachate. Elute with ethyl acetate after all the adsorption, concentrate and dry the eluent (about 500L) to obtain a dry paste of about 12kg, add 60L of acetonitrile to the dry paste to dissolve the crystals at 60°C, let stand at 15°C for 4h, and then filter with suction , the filter cake was dried to obtain 960 g of crude product, and the detected 10-DABⅢ content was 33.8%.

[0059] (3) Add 30 L of the treated blank reversed-phase stationary phase into a 300×600 high-pressure separation column (the treatment method of the ...

Embodiment 3

[0061] (1) Take 500kg of crushed European yew branches and leaves and pack them into 6m 3 In the diafiltration tank, add 0.5% acetic acid aqueous solution (temperature 40°C) for diafiltration, and mix the leachate in batches, with a total of about 9100m 3 , The effective amount of 10-DABⅢ detected by HPLC is about 601g.

[0062] (2) Adsorb the leachate after regeneration treatment of the resin used in Example 2 (resin regeneration treatment method is to first wash 2 column volumes with liquid caustic soda with a mass percentage concentration of 8%, and then rinse with drinking water until the effluent is neutral and wait use). Elute with ethyl acetate after all the adsorption, concentrate and dry the eluent (about 500L) to obtain a dry paste of about 18kg, add 54L of acetonitrile to the dry paste to dissolve the crystals at 70°C, let stand at 15°C for 4h, and then filter with suction , the filter cake was dried to obtain 1552 g of crude product, and the detected 10-DABⅢ cont...

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Abstract

The invention relates to a method for preliminarily separating 10-deacetyl baccatin III from Chinese yew branches and leaves. The method comprises the following steps of: performing percolation to extract crushed Chinese yew branches and leaves; then performing adsorption through a macroporous adsorption resin column, and performing elution by using an organic solvent; removing impurities to obtain a crude product of 10-deacetyl baccatin III; dissolving the crude product of 10-deacetyl baccatin III by using the organic solvent, and then adding a reverse phase filler to perform adsorption; putting the mixture into a preparation column, and then performing elution; and concentrating and removing impurities from a main section to obtain a pure product of 10-deacetyl baccatin III. According to the method, the use of a large amount of the organic solvent is not needed during extraction of the branches and leaves, the macroporous adsorption resin and a reverse phase filler can be repeatedly used, the type of the solvent is simplified, the operation is convenient to perform, the cost is lowered, and the recovery rate of 10-DAB III is higher. Meanwhile, low-content percolate during continuous production can be entirely recycled, so that the discharge and treatment of wastewater are reduced, and the method can be well applied in production.

Description

technical field [0001] The present invention relates to the extraction of yew plant components, in particular to a method for separating and purifying 10-deacetylbaccatin III from branches and leaves of yew. Background technique [0002] The molecular structure of 10-deacetylbaccatin III (10-DAB III) is as follows: [0003] [0004] 10-Deacetylbaccatin Ⅲ is the homologue of the anticancer drug taxol (Taxol). It is the main raw material for the synthesis of docetaxel and semi-synthetic paclitaxel. It mainly exists in the branches, leaves, roots and bark of Taxus chinensis. Paclitaxel or docetaxel has been clinically used in the treatment of breast cancer, ovarian cancer, lung cancer, etc., with good curative effect and low toxicity and side effects. The unique curative effect makes the market demand of this kind of drug increase day by day. However, due to the limitation of yew tree resources and the high cost of production input, the development of the natural paclitaxel...

Claims

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Application Information

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IPC IPC(8): C07D305/14
Inventor 任莉丁正飞胡立杨顺成喻琼林葛月兰
Owner 无锡紫杉药业股份有限公司
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