CN1295239C - Process for extracting camptothecin - Google Patents
Process for extracting camptothecin Download PDFInfo
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- CN1295239C CN1295239C CN 200410072869 CN200410072869A CN1295239C CN 1295239 C CN1295239 C CN 1295239C CN 200410072869 CN200410072869 CN 200410072869 CN 200410072869 A CN200410072869 A CN 200410072869A CN 1295239 C CN1295239 C CN 1295239C
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- camptothecin
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- aqueous ethanolic
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Abstract
The present invention relates to a method for extracting camptothecin. The present invention has the preparation steps that common camptotheca fruit is processed by diacolation or is processed by thermal extraction through an ethanol solution at a temperature of 25 to 80 DEG C; an extracting solution is introduced into a resin column with a macroporous resin (AL-2 adsorptive resin) and is adsorbed; then, the extracting solution is washed and desorbed by an ethanol aqueous solution; effluent is steamed, concentrated and recrystallized, etc. The rate of the raw material weight of common camptotheca fruit and the volume of resin is 2 to 4:1. the present invention has the advantages of simple technology, good product quality, high extraction rate, no three wastes, no environment pollution, wide raw material source, low cost and great economic benefit.
Description
Technical field
The present invention relates to the extracting method of macroporous adsorbent resin in traditional Chinese medicine ingredients separation, Application in Purification, particularly a kind of camptothecin.The present invention utilizes the macroporous resin chromatography, by simple production technique, obtains the camptothecin product of higher degree.
Technical background
Scientist has just found the existence of vincoside-lactam, but has not caused enough attention in the extraction separation research to camplotheca acuminata (Camptotheca) alkali.Vincoside-lactam has cytotoxic activity to the P388 white cell, does not study in great detail but its pharmaceutical use and clinical efficacy thereof done.According to the literature (Xu Rensheng, Zhao Zhiyuan, Lin Longze, chemical journal, 1977,35 (3,4): 193), the separation of vincoside-lactam can be adopted solvent extraction and alumina column chromatography method, the process complexity, yield is low.The report that utilizes multiple macroporous resin companion method purifying Fructus Camptothecae Acuminatae glycosides is also arranged in recent years, and (it is clear etc. that history is done for Wang Ruifang, Li Jiazheng.SCI, 2003,24 (8): 1534), but the increase of step has not only increased cost greatly, has also reduced productive rate.
Camptothecin, colourless needle, 210 ℃ of fusing points (decomposition), water insoluble and common organic solvents can be dissolved in methyl alcohol, propylene glycol and dimethyl sulfoxide (DMSO), and the placement gradual change is brown in air.Camptothecin has remarkable antitumour activity, and good water solubility, and toxic side effect is little, is expected to become a kind of important cancer therapy drug.
The Fructus Camptothecae Acuminatae powder adds in the hot alcohol extract, and the content of vincoside-lactam is far above camptothecine, and the content of camptothecin, in view of vincoside-lactam has antitumour activity and content is higher thereby has important research and development and is worth up to 0.27% in the Fructus Camptothecae Acuminatae.Separating vincoside-lactam in addition from Fructus Camptothecae Acuminatae also has great importance to the camplotheca acuminata resource that makes full use of China's abundant.
The chemosynthesis complex steps of camptothecin, yield are low, and no actual production is worth.The separation and purification camptothecin is expected to become the main stream approach of preparation camptothecin in the Fructus Camptothecae Acuminatae, and is convenient to industrial operation.About bibliographical information not being arranged so far by mentioning the separation camptothecin in the Fructus Camptothecae Acuminatae.
Summary of the invention
The extracting method that the purpose of this invention is to provide a kind of camptothecin, it is to utilize the macroporous resin adsorption chromatography by extraction separation camptothecin in the Fructus Camptothecae Acuminatae, to make full use of the camplotheca acuminata resource of China's abundant.Advantage of the present invention is that technology is simple, good product quality, and the extraction yield height, abundant raw material, cost is low, the no three wastes, free from environmental pollution, economic benefit is big.
Technical process of the present invention is: Fructus Camptothecae Acuminatae is pulverized the back and is extracted with aqueous ethanolic solution.Extracting solution concentrates through rotary evaporation, and cooled and filtered gets transparent crude extract.Dress AL-2 resin in exchange column is behind the Fructus Camptothecae Acuminatae extract upper prop, earlier with the prewashing of finite concentration aqueous ethanolic solution, to remove a large amount of impurity; Use the aqueous ethanolic solution drip washing of higher concentration again, get the camptothecin effluent liquid.The effluent liquid of camptothecin revolves to steam to be concentrated into separates out small amount of solid, places cooling and separates out a large amount of needle-like crystals, filters.Needle filters with 50% aqueous ethanolic solution ultrasonic dissolution, and filtrate is revolved inspissation and contracted, once more recrystallization.Repeatedly behind the recrystallization, crystal is become colorless by faint yellow.
The extracting method of camptothecin of the present invention is described in detail as follows: comprise the steps:
1) with the Fructus Camptothecae Acuminatae raw material pulverizing, extract with ethanolic soln diacolation or ethanolic soln heat, concentrate through rotary evaporation, be cooled to the room temperature after-filtration, get transparent extract.
2) will clarify extracting solution and feed in the resin column that macroporous adsorbent resin (AL-2 polymeric adsorbent, Tianjin Ourui Biology Technology Co., Ltd. produces) is housed and adsorb, with aqueous ethanolic solution washing and desorb; The flow velocity of absorption, washing, desorb be 0.5-2.5 bed volume/hour.
3) effluent liquid of camptothecin revolves to steam to be concentrated into and separates out small amount of solid, and placement is cooled to room temperature and separates out a large amount of needle-like crystals.
4) needle filters with 50% aqueous ethanolic solution ultrasonic dissolution, and filtrate is revolved inspissation and contracted, and recrystallization gets the camptothecin product once more.
It is 25-80 ℃ that described ethanolic soln heat is extracted.
The volume ratio of described Fructus Camptothecae Acuminatae raw material weight and resin is 2～4: 1, and gram: milliliter.
Described resin column footpath and post height ratio are 1: 5～30.
Described washings is the ethanol of 5%-35%, and described stripping liquid is the ethanolic soln of 40%-90%.
The present invention utilizes the macroporous resin adsorption chromatography by extraction separation camptothecin in the Fructus Camptothecae Acuminatae, has made full use of the camplotheca acuminata resource of China's abundant.Only, just can obtain pure product camptothecin product by " absorption---wash-out---recrystallization " simple production technique.Technology of the present invention is simple, good product quality, and the extraction yield height, abundant raw material, cost is low, the no three wastes, free from environmental pollution, economic benefit is big.
Embodiment:
Embodiment 1
Getting 20g Fructus Camptothecae Acuminatae pulverizing back extracts with 50 ℃ of heating of aqueous ethanolic solution of 50%.Extracting solution concentrates through rotary evaporation, is cooled to the room temperature after-filtration, gets transparent crude extract.Dress AL-2 resin 10mL in internal diameter is the exchange column of 1.5cm is behind the Fructus Camptothecae Acuminatae crude extract 300mL upper prop, earlier with the prewashing of 300mL30% aqueous ethanolic solution, to remove impurity; Use the aqueous ethanolic solution drip washing of 300mL50% again, get the camptothecin effluent liquid.The effluent liquid of camptothecin revolves to steam to be concentrated into separates out small amount of solid, and placement is cooled to room temperature and separates out a large amount of needle-like crystals, filters.Needle filters with 50% aqueous ethanolic solution ultrasonic dissolution, and filtrate is revolved inspissation and contracted, recrystallization once more, high-performance liquid chromatogram determination, camptothecin purity 98.6%.
Embodiment 2
Getting 10g Fructus Camptothecae Acuminatae pulverizing back extracts with 80 ℃ of heating of aqueous ethanolic solution of 50%.Extracting solution concentrates through rotary evaporation, and cooled and filtered gets transparent extract.Dress AL-2 polymeric adsorbent 7mL (wet bulb) in the exchange column of internal diameter 0.9cm, with the flow velocity upper prop (BV: bed volume) of purification liquid (105mL) with about 2BV/h, washing post with 2BV, use the drip washing of 150mL30% aqueous ethanolic solution again, use the aqueous ethanolic solution drip washing of 150mL50% again, get the camptothecin effluent liquid.The effluent liquid of camptothecin revolves to steam to be concentrated into separates out small amount of solid, places cooling and separates out a large amount of needle-like crystals, filters.Needle filters with 50% aqueous ethanolic solution ultrasonic dissolution, and filtrate is revolved inspissation and contracted, recrystallization once more, high-performance liquid chromatogram determination, camptothecin purity 99.0%.
Embodiment 3
Getting 200g Fructus Camptothecae Acuminatae pulverizing back extracts with 70 ℃ of heating of aqueous ethanolic solution of 70%.Extracting solution concentrates through rotary evaporation, and cooled and filtered gets transparent extract.Dress AL-2 polymeric adsorbent 100mL (wet bulb) in the exchange column of internal diameter 4cm, with the flow velocity upper prop (BV: bed volume) of purification liquid (1000mL) with about 2BV/h, washing post with 2BV, use the drip washing of 100mL30% aqueous ethanolic solution again, use the aqueous ethanolic solution drip washing of 150mL60% again, get the camptothecin effluent liquid.The effluent liquid of camptothecin revolves to steam to be concentrated into separates out small amount of solid, places cooling and separates out a large amount of needle-like crystals, filters.Needle filters with 50% aqueous ethanolic solution ultrasonic dissolution, and filtrate is revolved inspissation and contracted, recrystallization once more, high-performance liquid chromatogram determination, camptothecin purity 98.9%.
Claims (1)
1, a kind of extracting method of camptothecin, it is through following step:
1) with the Fructus Camptothecae Acuminatae raw material pulverizing, extract with ethanolic soln diacolation or ethanolic soln 25-80 ℃ of heat, concentrate through rotary evaporation, be cooled to the room temperature after-filtration, get transparent extract;
2) will clarify extracting solution and feed in the resin column that macroporous adsorbent resin is housed and adsorb, with aqueous ethanolic solution washing and desorb; The flow velocity of absorption, washing, desorb be 0.5-2.5 bed volume/hour; Described resin column footpath and post height ratio are 1: 5～30;
3) effluent liquid of camptothecin revolves to steam to be concentrated into and separates out small amount of solid, and placement is cooled to room temperature and separates out a large amount of needle-like crystals;
4) needle filters with 50% aqueous ethanolic solution ultrasonic dissolution, and filtrate is revolved inspissation and contracted, and recrystallization gets the camptothecin product once more; It is characterized in that:
Described macroporous adsorbent resin is the AL-2 polymeric adsorbent, and the volume ratio of described Fructus Camptothecae Acuminatae raw material weight and resin is 2～4: 1, and gram: milliliter.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410072869 CN1295239C (en) | 2004-11-25 | 2004-11-25 | Process for extracting camptothecin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410072869 CN1295239C (en) | 2004-11-25 | 2004-11-25 | Process for extracting camptothecin |
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| CN1634951A CN1634951A (en) | 2005-07-06 |
| CN1295239C true CN1295239C (en) | 2007-01-17 |
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| CN 200410072869 Expired - Fee Related CN1295239C (en) | 2004-11-25 | 2004-11-25 | Process for extracting camptothecin |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101313914B (en) * | 2007-05-29 | 2011-07-06 | 江苏康缘药业股份有限公司 | Uses and preparations of common camptotheca fruit glycosides of common camptotheca fruit extract |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100421564C (en) * | 2006-07-28 | 2008-10-01 | 浙江林学院 | Pesticide prepn produced with camptotheca material and its use |
| CN102786568B (en) * | 2012-07-26 | 2015-07-01 | 江苏康缘药业股份有限公司 | Vincoside lactam preparation method |
| CN103446172A (en) * | 2013-08-30 | 2013-12-18 | 苏州天南星生物科技有限公司 | Application of fructus camptothecae acuminatae extractive vincoside lactam |
| CN106518940B (en) * | 2016-11-07 | 2020-09-01 | 辽宁科技大学 | Method for purifying vincoside-lactam |
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- 2004-11-25 CN CN 200410072869 patent/CN1295239C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101313914B (en) * | 2007-05-29 | 2011-07-06 | 江苏康缘药业股份有限公司 | Uses and preparations of common camptotheca fruit glycosides of common camptotheca fruit extract |
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| Publication number | Publication date |
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| CN1634951A (en) | 2005-07-06 |
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