CN1472213A - High-performance camptothecin producing technology - Google Patents
High-performance camptothecin producing technology Download PDFInfo
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- CN1472213A CN1472213A CNA021327211A CN02132721A CN1472213A CN 1472213 A CN1472213 A CN 1472213A CN A021327211 A CNA021327211 A CN A021327211A CN 02132721 A CN02132721 A CN 02132721A CN 1472213 A CN1472213 A CN 1472213A
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Abstract
A process for effectively preparing camptothecine includes such steps as washing dendrophilous seeds, mixing with alcohol or acid-alcohol liquid, homogenizing, solid-liquid extracting, cavitation-cyclone for solid-liquid extracting, filtering, concentrating, cavitation-cyclone for liquid-liquid extracting, and purifying. Its advantages are high output rate and purity, short period and no pollution.
Description
Affiliated technical field:
The present invention relates to a kind of high-performance camptothecin producing technology, particularly a kind of employing homogenate extraction and cavitation DL extraction high-performance camptothecin producing technology.
Background technology:
At present, camptothecine and derivative thereof generally extract from Nyssaceae (Nyssaceae) plant camptotheca acuminata (Camptotheca acuminata) and obtain.
Current camptothecine extracting method has:
1, a kind of extracting method of camptothecine, Patent Office of the People's Republic of China's publication number: 1121920; Open day: 1996.05.08; Application number: 94111946.7, fruit or root skin that this invention relates to a kind of camplotheca acuminata are the processing method that raw material extracts camptothecine, adopt abrasive dust → poach → boil liquid to concentrate → paste → ethanol to separate gummy impurity → separate out crude product → chloroform mixed solution repeatedly to obtain the operational path of product behind the recrystallization, and in abrasive dust → poach operation, add oxidation inhibitor.The purity of drying products＞92%, output capacity is about 0.2 ‰.
2, a kind of production method Patent Office of the People's Republic of China publication number of camptothecine: 1251366; Open day: 2000.04.26; Application number: 99113256.4, it is raw material with leaf of Common Camptotheca and seed that this invention relates to a kind of, the processing method of production camptothecine.Behind raw material pulverizing → ethanol and water diacolation → concentrated percolate → macroporous adsorbent resin column chromatography → recrystallization, obtain the operational path of product.
3, a kind of production method Patent Office of the People's Republic of China publication number of camptothecine: 1239096; Open day: 1999.12.22; Application number: 99112767.6, this present invention relates to a kind of is main raw material with the leaf of Common Camptotheca, fruit is the processing method of auxiliary material production camptothecine.Obtain the operational path of product behind leftover materials after raw material pulverizing → ethanol percolation → supercritical carbon dioxide extraction diacolation extracts → concentrated percolate and the extraction liquid → macroporous adsorbent resin column chromatography → recrystallization.
The production method ubiquity of above-mentioned camptothecine that extraction time is longer, and extraction yield and yield are all lower, and production cost height, complex procedures are not easy to shortcomings such as popularization, and product yield only is 0.2～0.3 ‰.
Summary of the invention:
The object of the invention be to provide a kind of with short production cycle, extraction yield is high, product purity and the high high-performance camptothecin producing technology of yield.
In order to achieve the above object, the technical solution used in the present invention is:---------extracting solution concentrates---cavitation DL liquid-liquid extraction---purifying---finished product to cavitation DL liquid-solid extraction to the homogenate liquid-solid extraction to extract solvent with alcohol or acid alcohol behind the camptotheca seed cleaning removal impurity.
Advantage of the present invention is:
The present invention have with short production cycle, power consumption is few, environmentally safe.
2. advantages such as the present invention has replaced traditional material dry ground, heating is extracted or working methods such as mechanical stirring extraction and macroporous resin adsorption, countercurrent liquid-liquid extraction, and it is simple to have a technical process, and solvent load is few.
3. the camptothecine yield is 0.4～0.6 ‰, and purity is more than 98%.
Embodiment:
Below embodiments of the invention are described in further detail:
------------extracting solution concentrates---cavitation DL liquid-liquid extraction---purifying---finished product to cavitation DL liquid-solid extraction to the homogenate liquid-solid extraction in filtration to extract solvent with alcohol or acid alcohol behind the camptotheca seed cleaning removal impurity.
Described extraction solvent be 50～70% ethanol or 50～70% ethanol respectively with the mixed extraction solvent of 5～10% hydrochloric acid, 5～10% acetate or 5～10% propionic acid.
Described homogenate liquid-solid extraction is to adopt the raw material after cleaning to place hollander and paste roller mill to carry out the homogenate liquid-solid extraction simultaneously with extracting solvent, and making beating back raw meal particle size is 60～100 orders, and raw meal particle size is 150～200 orders behind the defibrination.
Described cavitation DL liquid-solid extraction is to place extractor to adopt the method for negative inspiratory pressure or malleation air inlet to carry out camptothecine respectively the material after the homogenate to extract, change extraction liquid extraction 2～3 times, 6～12 hours after-filtration of each extraction, united extraction liquid, negative pressure 0.06～0.1MPa, malleation 0.1～0.6MPa
Described filtration can be adopted respectively and hold back component 0.02～10 μ m particle, the multi-hole micro leaching film of negative pressure 0.06～0.1MPa carries out suction filtration, holds back component 0.02～10 μ m particle, the multi-hole micro leaching film of malleation 0.2～1MPa carries out press filtration or rotating speed 1800～2400r/min, and the whizzer of holding back component 0.02～10 μ m particle porous membrane carries out methods such as centrifuging.
It is to be 80～120 ℃ in temperature that described extracting solution concentrates, and negative pressure is to extract solvent recuperation under 0.06～0.1MPa or the condition of normal pressure.
The liquid-liquid extraction of described cavitation DL is that concentrated solution is mixed with the extraction agent equal-volume, can be under negative pressure 0.06～0.1MPa condition air-breathing or malleation be that cavitation DL liquid-liquid extraction 5～30min is carried out in 0.1～0.6MPa air inlet, extraction agent can adopt methylene dichloride or trichloromethane, the extraction liquid that leaves standstill behind the separatory carries out cavitation DL liquid-liquid extraction 5～30min with 5～10% hydrochloric acid or 5～10% acetate again, 5～10% hydrochloric acid or 5～10% acetic acid extraction liquid that leave standstill behind the separatory carry out the liquid-liquid extraction of 1～3 cavitation DL with methylene dichloride or trichloromethane again, each 5～30min, the extraction liquid that obtains methylene dichloride or trichloromethane is that 1～2 4～10% alcohol solvents carry out the liquid-liquid extraction of 1～3 cavitation DL again with PH again, each 5～30min, combined dichloromethane or chloroform extraction liquid are to carry out methylene dichloride under 45～70 ℃ of negative pressure condition that is 0.06～0.1MPa or chloroform extraction liquid concentrates in temperature.
Described purifying can adopt recrystallization or silica gel partition chromatography to carry out.
Embodiment 1:
Get camptotheca seed 70Kg and drop into hollander while mixing with 70% extraction using alcohol agent 300Kg, paste roller mill carries out the homogenate extraction, homogenate is squeezed into through underflow pump and is had that to hold back component be 0.02～10 μ m filter membrane, negative pressure is in the extractor of 0.1MPa, negative pressure cavitation DL extraction 6～12h, suction filtration, material extracts through the 70% ethanol 300Kg cavitation DL of PH=1 again, repeat this operation 2～3 times, merging filtrate, the camptothecine extraction yield is 0.8～1.2 ‰, filtrate is 80～120 ℃ through temperature, negative pressure is that 0.06～0.1MPa solvent recovery tower concentrates recovery ethanol, concentrated solution and equal-volume methylene dichloride or trichloromethane place extractor to carry out negative pressure cavitation DL liquid-liquid extraction 1～2 time, time is 5～10min/ time, the methylene dichloride or the chloroform extraction liquid that leave standstill behind the separatory are 45～50 ℃ through temperature again, negative pressure is that the solvent recuperation jar of 0.06～0.1MPa concentrates recovery methylene dichloride or trichloromethane, filter, filtrate is that 2 5% ethanol liquid carries out the negative pressure-cavitation homogenous solid-liquid phase extraction through PH again, get methylene dichloride or chloroform extraction liquid, leave standstill after the backflow put cold, it is 68.5g that crystallization gets crude product weight, purity 92%, getting finished product purity through recrystallization is more than 98.4%, weight is 34.25g, and yield is 0.5 ‰.
Embodiment 2:
Get camptotheca seed 70Kg and drop into hollander while mixing with the 70% extraction using alcohol agent 300Kg that acetate is modulated to PH=1, paste roller mill carries out the homogenate extraction, homogenate is squeezed into through underflow pump and is had that to hold back component be 0.02～10 μ m filter membrane, negative pressure is in the extractor of 0.1MPa, negative pressure cavitation DL extraction 6～12h, suction filtration, material extracts through the 70% ethanol 300Kg cavitation DL of PH=1 again, repeat this operation 2～3 times after, merging filtrate, this moment, the camptothecine extraction yield was 0.8～1.2 ‰, filtrate is 80～120 ℃ through temperature, negative pressure be 0.06～0.1MPa solvent recovery tower concentrate reclaim concentrated solution, concentrated solution places extractor to carry out negative pressure cavitation DL liquid-liquid extraction 1～2 time with equal-volume methylene dichloride or trichloromethane again, time is 5～10min/ time, the methylene dichloride or the chloroform extraction liquid that leave standstill behind the separatory are 45～50 ℃ through temperature again, negative pressure is that the solvent recuperation jar of 0.06～0.1MPa concentrates recovery methylene dichloride or trichloromethane, get methylene dichloride or trichloromethane concentrated solution, carrying out wash-out through the partition column chromatography of silica gel again separates, eluent adopts methylene dichloride or the absolute dichloromethane that contains 4～5% methyl alcohol, eluent reclaims and concentrates, and gets the camptothecine finished product.Finished product purity is 99.1%, and weight is 42.46g, and yield is 0.6 ‰.
Claims (8)
1. high-performance camptothecin producing technology is characterized in that: camptotheca seed extracts solvent with alcohol or acid alcohol after cleaning and removing impurity, and------cavitation DL liquid-solid extraction---filters that---extracting solution concentrates---cavitation DL liquid-liquid extraction---purifying---finished product to the homogenate liquid-solid extraction.
2, according to the described high-performance camptothecin producing technology of claim 1, it is characterized in that: described extraction solvent be 50～70% ethanol or 50～70% ethanol respectively with the mixed extraction solvent of 5～10% hydrochloric acid, 5～10% acetate or 5～10% propionic acid.
3, according to the described high-performance camptothecin producing technology of claim 1, it is characterized in that: described homogenate liquid-solid extraction is to adopt the camptotheca seed after cleaning to place hollander and paste roller mill to carry out the homogenate liquid-solid extraction simultaneously with the extraction solvent, making beating back raw meal particle size is 60～100 orders, and raw meal particle size is 150～200 orders behind the defibrination.
4, according to the described high-performance camptothecin producing technology of claim 1, it is characterized in that: described cavitation DL liquid-solid extraction is to place extractor to adopt negative pressure 0.06～0.1MPa method air-breathing or malleation 0.1～0.6MPa air inlet to carry out camptothecine respectively the material after the homogenate to extract, change extraction liquid extraction 2～3 times, 6～12 hours after-filtration of each extraction merge filtered liquid.
5, according to the described high-performance camptothecin producing technology of claim 1, it is characterized in that: filtration can be adopted respectively and hold back component 0.02～10 μ m particle, the multi-hole micro leaching film of negative pressure 0.06～0.1MPa carries out suction filtration, holds back component 0.02～10 μ m particle, the multi-hole micro leaching film of malleation 0.2～1MPa carries out press filtration or rotating speed 1800～2400r/min, and the whizzer of holding back component 0.02～10 μ m particle porous membrane carries out methods such as centrifuging.
6, according to the described high-performance camptothecin producing technology of claim 1, it is characterized in that: it is to be 80～120 ℃ in temperature that described extracting solution concentrates, and negative pressure is to extract solvent recuperation under 0.06～0.1MPa or the condition of normal pressure.
7, according to the described high-performance camptothecin producing technology of claim 1, it is characterized in that: the liquid-liquid extraction of described cavitation DL is that concentrated solution is mixed with the extraction agent equal-volume, can be under negative pressure 0.06～0.1MPa condition air-breathing or malleation be that cavitation DL liquid-liquid extraction 5～30min is carried out in 0.1～0.6MPa air inlet, extraction agent adopts methylene dichloride or trichloromethane, the extraction liquid that leaves standstill behind the separatory carries out cavitation DL liquid-liquid extraction 5～30min with 5～10% hydrochloric acid or 5～10% acetate again, 5～10% hydrochloric acid or 5～10% acetic acid extraction liquid that leave standstill behind the separatory carry out the liquid-liquid extraction of 1～3 cavitation DL with methylene dichloride or trichloromethane again, each 5～30min, the extraction liquid that obtains methylene dichloride or trichloromethane is that 1～2 4～10% alcohol solvents carry out the liquid-liquid extraction of 1～3 cavitation DL again with PH again, each 5～30min, obtaining methylene dichloride or chloroform extraction liquid, is to carry out methylene dichloride under 45～70 ℃ of negative pressure condition that is 0.06～0.1MPa or chloroform extraction liquid concentrates in temperature.
8, according to the described high-performance camptothecin producing technology of claim 1, it is characterized in that: purifying can adopt recrystallization or silica gel partition chromatography to carry out.
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| CNB021327211A CN1176087C (en) | 2002-07-30 | 2002-07-30 | High-performance camptothecin producing technology |
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| CNB021327211A CN1176087C (en) | 2002-07-30 | 2002-07-30 | High-performance camptothecin producing technology |
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| CN1176087C CN1176087C (en) | 2004-11-17 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006064517A3 (en) * | 2004-12-16 | 2007-07-05 | Cymbio Pharma Pvt Ltd | Methods for the purification of 20(s)-camptothecin |
| CN102093375A (en) * | 2011-02-28 | 2011-06-15 | 中国科学院过程工程研究所 | Method for extracting steam explosion common camptotheca fruits and preparing camptothecin |
| CN102093374A (en) * | 2010-11-30 | 2011-06-15 | 东北林业大学 | Method for efficiently extracting camptothecin derivative |
| CN102924376A (en) * | 2012-11-28 | 2013-02-13 | 云南省农业科学院药用植物研究所 | Method for preparing high-purity bulleyaconitine A |
| CN103975668A (en) * | 2014-03-30 | 2014-08-13 | 东北林业大学 | Method for improving content of 10-methoxycamptothecine in Camptotheca acuminata seeds |
| WO2017157292A1 (en) * | 2016-03-16 | 2017-09-21 | 科沃斯机器人股份有限公司 | Anti-static vacuum cleaner |
-
2002
- 2002-07-30 CN CNB021327211A patent/CN1176087C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006064517A3 (en) * | 2004-12-16 | 2007-07-05 | Cymbio Pharma Pvt Ltd | Methods for the purification of 20(s)-camptothecin |
| CN102093374A (en) * | 2010-11-30 | 2011-06-15 | 东北林业大学 | Method for efficiently extracting camptothecin derivative |
| CN102093375A (en) * | 2011-02-28 | 2011-06-15 | 中国科学院过程工程研究所 | Method for extracting steam explosion common camptotheca fruits and preparing camptothecin |
| CN102924376A (en) * | 2012-11-28 | 2013-02-13 | 云南省农业科学院药用植物研究所 | Method for preparing high-purity bulleyaconitine A |
| CN102924376B (en) * | 2012-11-28 | 2014-10-29 | 云南省农业科学院药用植物研究所 | Method for preparing high-purity bulleyaconitine A |
| CN103975668A (en) * | 2014-03-30 | 2014-08-13 | 东北林业大学 | Method for improving content of 10-methoxycamptothecine in Camptotheca acuminata seeds |
| CN103975668B (en) * | 2014-03-30 | 2015-03-25 | 东北林业大学 | Method for improving content of 10-methoxycamptothecine in Camptotheca acuminata seeds |
| WO2017157292A1 (en) * | 2016-03-16 | 2017-09-21 | 科沃斯机器人股份有限公司 | Anti-static vacuum cleaner |
| US11013386B2 (en) | 2016-03-16 | 2021-05-25 | Tineco Intelligent Technology Co., Ltd. | Anti-static vacuum cleaner |
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| CN1176087C (en) | 2004-11-17 |
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