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Method for extracting 10-deacetyl baccatin III from branches and leaves of taxus chinensis

A technology of yew branches and leaves and acetyl bacca, which is applied in the field of extraction of medicinal compounds to achieve the effects of reducing losses, shortening the process flow, and shortening the extraction time

Inactive Publication Date: 2011-04-20
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

[0006] The technical problem to be solved by the present invention is to overcome the defects of the existing methods for extracting 10-deacetylbaccatin III from branches and leaves of Taxus chinensis, and provide an extraction and purification method with good product quality, high yield and low cost

Method used

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  • Method for extracting 10-deacetyl baccatin III from branches and leaves of taxus chinensis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] 1. Take 100kg of artificially planted southern yew branches and leaves, crush them into 20-mesh powder, put them into an ultrasonic tank, add 100L of water at the same time, ultrasonicate at 60°C for half an hour, and filter. Add 60L, 30L, and 30L dichloromethane three times for extraction, combine the dichloromethane phases and concentrate to obtain 310.7g of extract, with a content of 2.58%.

[0016] 2. Add 310.0g of extract to 310ml of acetonitrile, and heat to 50-80°C in a water bath to dissolve. Put in -10°C environment for 24 hours, filter the crystals, and dry at low temperature to obtain 29.58g of white powder with a content of 24.92%.

[0017] 3. Dissolve 29.08g of 24.92% white powder with 580ml of dichloromethane:methanol (volume ratio 4:1) at 50°C, cool to -10°C, filter, and dry at low temperature to obtain 7.77g of white powder. 80.28%.

[0018] 4.7.67g of white powder with a content of 80.28%, heated and dissolved with 190ml of dichloromethane:methanol (1...

Embodiment 2

[0022] 1. Take 100kg of artificially planted southern yew branches and leaves, crush them into 20-mesh powder, put them into an ultrasonic tank, add 200L of water at the same time, ultrasonicate at 60°C for half an hour, and filter. Add 80L, 30L, and 20L dichloromethane three times for extraction, combine the dichloromethane phases and concentrate to obtain 312.3g of extract, with a content of 2.88%.

[0023] 2. Add the extract to 900ml of acetonitrile, and heat it in a water bath to 50-80°C to dissolve. Put in -10°C environment for 24 hours, filter the crystals, and dry at low temperature to obtain 30.27g of white powder with a content of 25.01%.

[0024] 3. Dissolve 30.17g of 25.01% white powder with 600ml of dichloromethane:methanol (volume ratio 4:1) at 50°C, cool to -10°C, filter, and dry at low temperature to obtain 8.03g of white powder. 81.31%.

[0025] 4. 7.93g of white powder with a content of 81.31% was dissolved by heating at 50°C with 190ml of dichloromethane:me...

Embodiment 3

[0029] 1. Take 100kg of artificially planted southern yew branches and leaves, crush them into 20-mesh powder, put them into an ultrasonic tank, add 300L of water at the same time, ultrasonicate at 60°C for half an hour, and filter. Add 70L, 50L, and 30L dichloromethane three times for extraction, combine the dichloromethane phases and concentrate to obtain 325.9 g of extract, with a content of 2.57%.

[0030] 2. Add the extract to 600ml of acetonitrile, and heat it in a water bath to 50-80°C to dissolve. Put in -10°C environment for 24 hours, filter the crystals, and dry at low temperature to obtain 29.92g of white powder with a content of 25.52%.

[0031] 3. Dissolve 29.82g of 25.52% white powder with 600ml of dichloromethane:methanol (volume ratio 4:1) at 50°C, cool to -10°C, filter, and dry at low temperature to obtain 7.82g of white powder. 81.59%.

[0032] 4. 7.72g of white powder with a content of 81.59% was dissolved by heating at 50°C with 190ml of dichloromethane:m...

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Abstract

The invention discloses a method for extracting 10-eacetyl baccatin III from branches and leaves of taxus chinensis, comprising the following steps: 1, extraction and concentration: proportionally mixing smashed branches and leaves of taxus chinensis with water, carrying out ultrasonic extraction, adding solvent into filtrate obtained from ultrasonic extraction to extract, and concentrating extract liquor to obtain extract; and 2, recrystallization: firstly dissolving the extract into acetonitrile by heating, cooling and crystallizing, and filtering to obtain the crystalline powder of 10-eacetyl baccatin III. In the invention, the method for extracting and preparing 10-eacetyl baccatin III with high content, high yield and low cost is provided.

Description

technical field [0001] The invention relates to a chemical extraction method, in particular to an extraction method of medicinal compounds. Background technique [0002] 10-Deacetylbaccatin Ⅲ (10-DABⅢ) is a natural organic compound isolated from Taxus chinensis, which is used to synthesize paclitaxel or docetaxel. Its molecular structure is as follows: [0003] [0004] Paclitaxel is also a natural organic compound found in the branches and leaves of yew. It has a strong killing effect on breast cancer, ovarian cancer, lung cancer and leukemia cells. It is one of the effective anticancer drugs, and its demand occupies a large proportion in the existing antineoplastic drug market. However, the source of natural paclitaxel is extremely limited at present, the content in the bark is 0.01%-0.03%, and the yew grows very slowly. Therefore, researchers have successfully used 10DAB in yew to semi-synthesize paclitaxel to expand the source of paclitaxel. However, how to obtain ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D305/14
Inventor 张永兵卢定强徐信保李隆黄辉周理洁尤新晨
Owner 无锡紫杉药业股份有限公司
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