CN107056866A - A kind of method for obtaining Cucurbitacin B - Google Patents
A kind of method for obtaining Cucurbitacin B Download PDFInfo
- Publication number
- CN107056866A CN107056866A CN201710194318.1A CN201710194318A CN107056866A CN 107056866 A CN107056866 A CN 107056866A CN 201710194318 A CN201710194318 A CN 201710194318A CN 107056866 A CN107056866 A CN 107056866A
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- CN
- China
- Prior art keywords
- cucurbitacin
- ethanol
- extracted
- ethyl acetate
- separate out
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
Abstract
The invention belongs to field of natural medicinal chemistry, it is characterised in that：Take Tibet picrorhiza rhizome pulverizing medicinal materials, plus 75% 95% alcohol reflux of 16 20 times of amounts is extracted 23 times, ethanol is recovered under reduced pressure in extract solution, and concentrate is extracted with ethyl acetate, and takes organic layer.Ethyl acetate is reclaimed to be concentrated.Concentration volume to glass bar, which is dipped, slightly to be sticked.Placed 24 hours under the conditions of 10 DEG C 5 DEG C, separate out crystallization, filtering, crystalline solid adds 95% ethanol and carries out backflow dissolving.Place, separate out crystallization, be filtrated to get Cucurbitacin B.Cucurbitacin B is prepared using this technique.Technique is simple, and cost is small, and yield is high, and content is high.It is adapted to industrial-scale production.
Description
Technical field
The invention belongs to field of natural medicinal chemistry, it is related to a kind of using extraction and recrystallization technology purifying Cucurbitacin B
Method.
Background technology
Tibet picrorhiza rhizome is the dry rhizome of goatweed Radix picrorrhizae, there is heat-clearing, dehumidifying, improving eyesight, hepatic cholagogic, treatment
Main component in pediatric epilepsy scared, infantile malnutrition due to digestive disturbances or intestinalparasites, rush down dysentery, Radix picrorrhizae is iridoids, cucurbitacine and phenolic glycoside class.
Isolate the compositions such as Cucurbitacin B, E the domestic beginning of the seventies from Chinese medicine muskmelon pedicel, and carry out antitumor, immune increase
The pharmacological researches such as strong and anti-hepatitis.The pharmacological action of report has：Cell toxicant and antitumaous effect；Anti- chemical carcinogenesis；It is liver protection, anti-
Hepatitis is acted on；Improve immunologic function；To cardiovascular effect；Anti-inflammatory；Suppress the effect of hepatic fibroplasia；In addition with stimulation stomach
Bowel movement, can also practise contraception.
The document report of clinical research：Cucurbitacin has cell toxicant and antitumor, liver protection, anti-hepatitis, improves immunologic function,
Anti- chemical tumorigenesis, increases capillary permeability, the effect of stimulating gastrointestinal road.
The content of the invention
It is an object of the invention to be to solve shortcomings and deficiencies of the prior art, a kind of obtained Cucurbitacin B is added
Method.
A kind of method for obtaining Cucurbitacin B, it is characterised in that：Take Tibet picrorhiza rhizome pulverizing medicinal materials, plus 16-20 times is measured
75%-95% alcohol reflux is extracted 2-3 times, and ethanol is recovered under reduced pressure in extract solution, and concentrate is extracted with ethyl acetate, and takes organic layer.
Ethyl acetate is reclaimed to be concentrated.Concentration volume to glass bar, which is dipped, slightly to be sticked.- 10 DEG C -- place 24 hours, separate out under the conditions of 5 DEG C
Crystallization, filtering, crystalline solid adds 95% ethanol and carries out backflow dissolving.Place, separate out crystallization, be filtrated to get Cucurbitacin B.Using
This technique prepares Cucurbitacin B
Medicinal material used is Tibet picrorhiza rhizome；Described reflux temperature is 70-100 DEG C.
It is an advantage of the present invention that using conventional method, cost is low, simple to operate, is particularly suitable for use in heavy industrialization
Production.
Embodiment 1：
Following examples are illustrated to the present invention, but the scope of the present invention is not limited to the content that the following example is included.
1. the Tibet picrorhiza rhizome medicinal material for taking 100g to crush, with 95% ethanol 2000ml refluxing extractions 3 times, volume is respectively
800ml, 600ml, 600ml.
It is about 120ml to volume 2. extract solution is concentrated under reduced pressure, is extracted with 900ml ethyl acetate, points 3 times, often
Secondary volume is 300ml, combining extraction liquid, and is concentrated, to about 50ml.
3. an above-mentioned concentrate is put into 0 DEG C of refrigerator and stands 24 hours, treat that its crystallization is complete, filtering.
4. an above-mentioned crystalline solid is transferred in round-bottomed flask, and adds 80ml, 95% ethanol carries out backflow dissolving, treats that its is complete
Taken out after fully dissolved, place, treat that it separates out crystallization again, filtering is produced.
5. drying to obtain 4.1g, and detected with efficient liquid phase, and national standard material（Cucurbitacin B）Compare, be defined as
Cucurbitacin B.
Embodiment 2：
Following examples are illustrated to the present invention, but the scope of the present invention is not limited to the content that the following example is included
The Tibet picrorhiza rhizome medicinal material that 100g is crushed is taken, with 90% ethanol 2000ml refluxing extractions 3 times, volume is 800ml respectively,
600ml, 600ml.
It is about 120ml to volume 2. extract solution is concentrated under reduced pressure, is extracted with 900ml ethyl acetate, points 3 times, often
Secondary volume is 300ml, combining extraction liquid, and is concentrated, to about 50ml.
3. an above-mentioned concentrate is put into 0 DEG C of refrigerator and stands 24 hours, treat that its crystallization is complete, filtering.
4. an above-mentioned crystalline solid is transferred in round-bottomed flask, and adds 80ml, 95% ethanol carries out backflow dissolving, treats that its is complete
Taken out after fully dissolved, place, treat that it separates out crystallization again, filtering is produced.
5. drying to obtain 3.9g, and detected with efficient liquid phase, and national standard material（Cucurbitacin B）Compare, be defined as
Cucurbitacin B.
Claims (3)
1. Tibet picrorhiza rhizome pulverizing medicinal materials are taken, plus the 16-20 times of 75%-95% measured alcohol reflux is extracted 2-3 times, extract solution decompression
Ethanol is reclaimed, concentrate is extracted with ethyl acetate, and takes organic layer；Ethyl acetate is reclaimed to be concentrated；Concentration volume is to glass bar
Dip and slightly stick；- 10 DEG C -- placed 24 hours under the conditions of 5 DEG C, separate out crystallization, filtering, crystalline solid adds 95% ethanol and flowed back
Dissolving；Place, separate out crystallization, be filtrated to get Cucurbitacin B.
2. the method for Cucurbitacin B is obtained as claimed in claim 1, it is characterised in that medicinal material used is Tibet picrorhiza rhizome.
3. the method for Cucurbitacin B is obtained as claimed in claim 1, it is characterised in that described reflux temperature is 70-100 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710194318.1A CN107056866A (en) | 2017-03-28 | 2017-03-28 | A kind of method for obtaining Cucurbitacin B |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710194318.1A CN107056866A (en) | 2017-03-28 | 2017-03-28 | A kind of method for obtaining Cucurbitacin B |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107056866A true CN107056866A (en) | 2017-08-18 |
Family
ID=59617996
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710194318.1A Pending CN107056866A (en) | 2017-03-28 | 2017-03-28 | A kind of method for obtaining Cucurbitacin B |
Country Status (1)
| Country | Link |
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| CN (1) | CN107056866A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112972546A (en) * | 2019-12-16 | 2021-06-18 | 鲁南制药集团股份有限公司 | Preparation containing rhizoma picrorhizae effective part and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101103989A (en) * | 2006-07-10 | 2008-01-16 | 博仲盛景医药技术（北京）有限公司 | Medicinal composition for promoting enterogastric peristalsis |
| CN101759746A (en) * | 2009-11-24 | 2010-06-30 | 浙江工业大学 | Method for extracting and separating cucurbitacin B |
| CN101974055A (en) * | 2010-07-26 | 2011-02-16 | 南京泽朗农业发展有限公司 | Method for extracting cucurbitacin B |
| CN103992366A (en) * | 2014-05-13 | 2014-08-20 | 天津药物研究院 | A method of preparing cucurbitacin B |
| CN104086613A (en) * | 2014-07-21 | 2014-10-08 | 西安天丰生物科技有限公司 | Method for separating cucurbitacin B from muskmelon vine by virtue of catalytic reaction |
-
2017
- 2017-03-28 CN CN201710194318.1A patent/CN107056866A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101103989A (en) * | 2006-07-10 | 2008-01-16 | 博仲盛景医药技术（北京）有限公司 | Medicinal composition for promoting enterogastric peristalsis |
| CN101759746A (en) * | 2009-11-24 | 2010-06-30 | 浙江工业大学 | Method for extracting and separating cucurbitacin B |
| CN101974055A (en) * | 2010-07-26 | 2011-02-16 | 南京泽朗农业发展有限公司 | Method for extracting cucurbitacin B |
| CN103992366A (en) * | 2014-05-13 | 2014-08-20 | 天津药物研究院 | A method of preparing cucurbitacin B |
| CN104086613A (en) * | 2014-07-21 | 2014-10-08 | 西安天丰生物科技有限公司 | Method for separating cucurbitacin B from muskmelon vine by virtue of catalytic reaction |
Non-Patent Citations (1)
| Title |
|---|
| 王答祺等: "西藏胡黄连的化学成分", 《云南植物研究》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112972546A (en) * | 2019-12-16 | 2021-06-18 | 鲁南制药集团股份有限公司 | Preparation containing rhizoma picrorhizae effective part and preparation method thereof |
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Application publication date: 20170818 |
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