CN101289452A - Process for abstracting camptothecine form nothapodytes - Google Patents
Process for abstracting camptothecine form nothapodytes Download PDFInfo
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- CN101289452A CN101289452A CNA2008100287400A CN200810028740A CN101289452A CN 101289452 A CN101289452 A CN 101289452A CN A2008100287400 A CNA2008100287400 A CN A2008100287400A CN 200810028740 A CN200810028740 A CN 200810028740A CN 101289452 A CN101289452 A CN 101289452A
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Abstract
The invention relates to a method for extracting camptothecin from osmyl horse hiki, which adopts the following technical proposal: fresh osmyl horse hiki leaves are selected; the osmyl horse hiki leaves are dried; the osmyl horse hiki leaves are grinded; extract ethanol is added in the ground materials and extraction is carried out by heating; the extract and branch leaves slag are caused to be separated after being filtered; the extract is concentrated to obtain a concentrate; the concentrate is extracted by using a extractant which is recovered to obtain an extracted concentrate; and the extracted concentrate is purified to obtain a finished product. The method has the advantages of a higher purity of the finished product up to more than 99 percent, a larger quantity of finished products and the lower production cost. Meanwhile, the method improves the production efficiency and is characterized by saving energy and protecting environment.
Description
Technical field
The present invention relates to a kind of method of extracting camptothecine, particularly a kind of method of from form nothapodytes, extracting camptothecine.
Background technology
Existing anticancer bulk drug-camptothecine, all be from the fruit of camplotheca acuminata, to extract, because the growth cycle of camplotheca acuminata is very long, 8-15 ability result, and content of camptothecine is extremely low in it, content has only 1/10000ths, and the form nothapodytes of utilization high-tech means artificial growth, in it content of camptothecine up to 2/10000ths. 35, thereby in the process of extracting, cause production cost height, extraction yield and production efficiency extremely low, the purity of the finished product of output is not high.
Summary of the invention
The object of the present invention is to provide a kind of from form nothapodytes, extract camptothecine and can make the purity of camptothecine higher, the method for from form nothapodytes, extracting camptothecine that output is bigger.
The present invention is by the following technical solutions:
A. choose fresh form nothapodytes branches and leaves;
B. dry form nothapodytes branches and leaves;
C. pulverize the form nothapodytes branches and leaves;
D. add extracting solution ethanol in the raw material after pulverizing, heating is extracted;
E. filter, extracting solution is separated with the branches and leaves slag;
F. concentrated extracting solution obtains enriched material;
G. with extraction agent enriched material is extracted, and reclaim extraction agent, obtain extracting enriched material;
H. the extraction enriched material is carried out purifying;
I. obtain finished product.
Advantage of the present invention is:
The purity of finished product is higher, and purity is more than 99%; The output of producing is bigger; Reduce production cost, improved production efficiency; Characteristics with energy-conserving and environment-protective.
Embodiment
Below embodiments of the invention are further described:
A. choose fresh form nothapodytes branches and leaves;
B. dry form nothapodytes branches and leaves;
C. pulverize the form nothapodytes branches and leaves, with pulverizing mill the form nothapodytes branches and leaves are pulverized, the granular size after the pulverizing reaches more than 80 orders.；
D. add extracting solution ethanol in the raw material after will pulverizing, its solid-liquid ratio is 3: 1, adds extraction heat, and temperature is controlled between 40-75 ℃, and camptothecine is entered in the ethanol extract;
E. filter, extracting solution is separated with the branches and leaves slag;
F. concentrated extracting solution is to be 0.3-0.8Mpa in negative pressure, and temperature is carried out alcoholic acid and reclaimed under 60-80 ℃ condition, obtain containing the enriched material of camptothecine;
G. when enriched material is extracted, the extraction agent that is adopted is sherwood oil or methylene dichloride, sherwood oil or methylene dichloride are mixed with the enriched material equal-volume, after leaving standstill separatory, obtain sherwood oil or dichloromethane extraction liquid, sherwood oil or dichloromethane extraction liquid are 0.1-0.2Mpa in negative pressure, and temperature is under 60-80 ℃ condition, reclaim sherwood oil or methylene dichloride, obtain extracting enriched material;
H. the method that the extraction enriched material is carried out purifying is:
A, at first adopt silica gel column chromatography, preliminary crystallization purity reaches about 70%;
B, secondly carry out low pressure column chromatography, crystallization purity reaches about 80%;
C, carry out the FLASH medium pressure column chromatography then, crystallization purity reaches about 95%;
D, carry out recrystallization at last, its purity reaches more than 99%.
I, obtain finished product.
Claims (6)
1, a kind of method of extracting camptothecine from form nothapodytes is characterized in that:
A. choose fresh form nothapodytes branches and leaves;
B. dry form nothapodytes branches and leaves;
C. pulverize the form nothapodytes branches and leaves;
D. add extracting solution ethanol in the raw material after pulverizing, heating is extracted;
E. filter, extracting solution is separated with the branches and leaves slag;
F. concentrated extracting solution obtains enriched material;
G. with extraction agent enriched material is extracted, and reclaim extraction agent, obtain extracting enriched material;
H. the extraction enriched material is carried out purifying;
I. obtain finished product.
2, the method for extracting camptothecine from the form nothapodytes branches and leaves according to claim 1, it is characterized in that: with pulverizing mill the form nothapodytes branches and leaves are pulverized, the granular size after the pulverizing reaches more than 80 orders.
3, the method for from the form nothapodytes branches and leaves, extracting camptothecine according to claim 1, it is characterized in that: add extracting solution ethanol in the raw material after pulverizing, its solid-liquid ratio is 3: 1, and heating is extracted, temperature is controlled between 40-75 ℃, and camptothecine is entered in the ethanol extract.
4, the method for extracting camptothecine from the form nothapodytes branches and leaves according to claim 1 is characterized in that: concentrated extracting solution is to be 0.3-0.8Mpa in negative pressure, and temperature carries out alcoholic acid is reclaimed under 60-80 ℃ condition.
5, the method for from the form nothapodytes branches and leaves, extracting camptothecine according to claim 1, it is characterized in that: the extraction agent that enriched material is extracted adopts sherwood oil or methylene dichloride, sherwood oil or methylene dichloride are mixed with the enriched material equal-volume, after leaving standstill separatory, obtain sherwood oil or dichloromethane extraction liquid, sherwood oil or dichloromethane extraction liquid are 0.1-0.2Mpa in negative pressure, and temperature is under 60-80 ℃ condition, reclaim sherwood oil or methylene dichloride, obtain extracting enriched material.
6, the method for extracting camptothecine from the form nothapodytes branches and leaves according to claim 1 is characterized in that: the method for the extraction enriched material being carried out purifying is:
A, at first adopt silica gel column chromatography, preliminary crystallization purity reaches about 70%;
B, secondly carry out low pressure column chromatography, crystallization purity reaches about 80%;
C, carry out the FLASH medium pressure column chromatography then, crystallization purity reaches about 95%;
D, carry out recrystallization at last, its purity reaches more than 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100287400A CN101289452A (en) | 2008-06-12 | 2008-06-12 | Process for abstracting camptothecine form nothapodytes |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100287400A CN101289452A (en) | 2008-06-12 | 2008-06-12 | Process for abstracting camptothecine form nothapodytes |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101289452A true CN101289452A (en) | 2008-10-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100287400A Pending CN101289452A (en) | 2008-06-12 | 2008-06-12 | Process for abstracting camptothecine form nothapodytes |
Country Status (1)
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| CN (1) | CN101289452A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071233A (en) * | 2010-12-06 | 2011-05-25 | 张苑金 | Technical method for synthesizing camptothecin through artificial induction of nothapodytes nimmoniana (graham) mablerley endophytes |
| CN102603758A (en) * | 2012-02-12 | 2012-07-25 | 张苑金 | Extraction method of camptothecin and 9-hydroxymethyl camptothecin from tender leaves and twigs of Nothapodytes nimmoniana |
| CN102603757A (en) * | 2012-01-17 | 2012-07-25 | 花垣恒远植物生化有限责任公司 | Method for extracting and separating camptothecin from Nothapodytes pittosporoides (Oliv.) Sleum. |
| CN103181272A (en) * | 2011-12-28 | 2013-07-03 | 广东神农衍生物科技有限公司 | Artificial planting method for medical raw materials of nothapodytes nimmoniana |
| CN103664975A (en) * | 2012-09-19 | 2014-03-26 | 西安博爱制药有限责任公司 | Method of extracting camptothecin in nothapodytes pittosporoides |
| CN104619322A (en) * | 2013-07-24 | 2015-05-13 | 张苑金 | Anticancer pharmaceutical composition, preparation method for same, and use thereof |
| CN108283606A (en) * | 2018-04-16 | 2018-07-17 | 广东奇化化工交易中心股份有限公司 | Nti-freckle daily chemical products and preparation method thereof made of a kind of mappia foetida extract |
-
2008
- 2008-06-12 CN CNA2008100287400A patent/CN101289452A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102071233A (en) * | 2010-12-06 | 2011-05-25 | 张苑金 | Technical method for synthesizing camptothecin through artificial induction of nothapodytes nimmoniana (graham) mablerley endophytes |
| CN103181272A (en) * | 2011-12-28 | 2013-07-03 | 广东神农衍生物科技有限公司 | Artificial planting method for medical raw materials of nothapodytes nimmoniana |
| CN102603757A (en) * | 2012-01-17 | 2012-07-25 | 花垣恒远植物生化有限责任公司 | Method for extracting and separating camptothecin from Nothapodytes pittosporoides (Oliv.) Sleum. |
| CN102603758A (en) * | 2012-02-12 | 2012-07-25 | 张苑金 | Extraction method of camptothecin and 9-hydroxymethyl camptothecin from tender leaves and twigs of Nothapodytes nimmoniana |
| CN103664975A (en) * | 2012-09-19 | 2014-03-26 | 西安博爱制药有限责任公司 | Method of extracting camptothecin in nothapodytes pittosporoides |
| CN104619322A (en) * | 2013-07-24 | 2015-05-13 | 张苑金 | Anticancer pharmaceutical composition, preparation method for same, and use thereof |
| CN108283606A (en) * | 2018-04-16 | 2018-07-17 | 广东奇化化工交易中心股份有限公司 | Nti-freckle daily chemical products and preparation method thereof made of a kind of mappia foetida extract |
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Open date: 20081022 |