CN102030758A - Preparation method of chalepensin - Google Patents
Preparation method of chalepensin Download PDFInfo
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- CN102030758A CN102030758A CN2010105541320A CN201010554132A CN102030758A CN 102030758 A CN102030758 A CN 102030758A CN 2010105541320 A CN2010105541320 A CN 2010105541320A CN 201010554132 A CN201010554132 A CN 201010554132A CN 102030758 A CN102030758 A CN 102030758A
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- chalepensin
- ethanol
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- zhong
- microwave extracting
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Abstract
The invention relates to a chalepensin preparation method with simple operation, less pollution and less energy consumption. The processing steps comprises the steps: taking clausena lansium velamen; adding 70-90% of ethanol; carrying out microwave extraction in a microwave extraction device; merging extract liquors; filtering, carrying out reduced pressure recovery on recycle ethanol, and concentrating; carrying out multistage countercurrent extraction by acetone-water mixed solvent at the ratio of 5: 1, merging extract liquors, adding the extract liquor onto a macroporous absorption resin column to be absorbed, eluting by the ethanol, collecting elute, recycling the ethanol under reduced pressure, concentrating, adding normal hexane for crystallization, separating crystals, and washing and drying. The chalepensin prepared by the invention has high purity, and industrialization amplifying is easy to realize.
Description
Technical field
The present invention relates to the preparation method of Yi Zhong chalepensin, especially a kind of from plant the preparation method of Ti Qu chalepensin.
Background technology
Chalepensin (Chalepensin), molecular formula: C
16H
14O
3, molecular weight: 254.285, CAS accession number: 13164-03-9.Mainly be present in the Rutaceae various plants, wherein content is higher in rutaceae Calusena lansium Clausena lansium (Lour.) the Skeels root skin, and raw material sources are abundant.Its molecular formula is as follows:
Modern study shows that the ， chalepensin has antifertility, calcium antagonism isoreactivity, and it is also as the raw material that synthesizes other reactive derivative simultaneously.
The velamen of rutaceae Calusena lansium Clausena lansium (Lour.) Skeels uses as the Chinese medicine Radix clausenae lansii, has the effect of promoting the circulation of QI to relieve pain.
In the prior art, still be not applicable to preparation technology's report of Gao Chun Du chalepensin industrialized production.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, product purity Gao De chalepensin.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the Radix clausenae lansii skin, add the 70-90% ethanol that its quality 6-10 doubly measures, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300-600W extracts 1-3 time, each 3-10 minute, combining extraction liquid filters, and decompression recycling ethanol also concentrates, concentrating with ratio is that 5: 1 acetone-water mixed solvent carries out the 3-6 stage countercurrent and extracts, the volume ratio of concentrated solution and the total consumption of mixed solvent is 1: 3-6, and combining extraction liquid joins on the macroporous adsorptive resins and adsorbs, the 40-60% ethanol elution, collect 3-8 and doubly measure the column volume elutriant, decompression recycling ethanol also concentrates, and adds the normal hexane crystallization, fractional crystallization, washing, be drying to obtain.
Microwave extracting is preferably 80% with concentration of ethanol, and consumption is preferably 8 times of amount volumes of raw materials quality.
The power of microwave extracting is preferably 500W.
The number of times of microwave extracting is preferably 2 times, each 8 minutes.
The progression of counter-current extraction is preferably 5 grades, and the volume ratio of concentrated solution and the total consumption of mixed solvent is 1: 5.
Macroporous adsorbent resin is selected from a kind of in D101 type, D102 type, the AB8 type macroporous adsorbent resin.
Macroporous adsorbent resin wash-out concentration of ethanol is 50%.
The macroporous adsorbent resin wash-out is 5 times of amount column volumes with the alcoholic acid collecting amount.
Preparation Suo De chalepensin can adopt following method to detect:
Test example 1 HPLC method Ce is Dinged chalepensin purity
Chromatographic condition
Chromatographic column: octadecylsilane bonding glue silica gel is weighting agent; Moving phase: methanol-water solution (90: 10); Flow velocity: 1.0mL/min; Detect wavelength: 330nm; Column temperature: 30 ℃.
Measuring method
Accurate Cheng Qu chalepensin 2mg places the 50mL measuring bottle, adds people's methyl alcohol 20mL, and sonic oscillation makes dissolving, and methanol constant volume is drawn 10 μ L to scale, injects high performance liquid chromatograph, adopts normalization method working sample purity.
Adopt Zhi Bei chalepensin of the present invention, be beneficial to big production operation, energy consumption is little, pollutes little.
The present invention is further elaborated below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get Radix clausenae lansii skin 10Kg, 70% ethanol that adds 60L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300W extracts 3 minutes 1 time, get extraction liquid, filter, decompression recycling ethanol also concentrates, and concentrating with ratio is that 5: 1 acetone-water mixed solvent carries out 3 stage countercurrents and extracts, the volume ratio of concentrated solution and the total consumption of mixed solvent is 1: 3, combining extraction liquid joins on the D101 type macroporous adsorptive resins and adsorbs 40% ethanol elution, collect 3 times of amount column volume elutriants, decompression recycling ethanol also concentrates, and adds the normal hexane crystallization, fractional crystallization, washing, be drying to obtain white platelet chalepensin 5.6g, detect through HPLC, purity is 95.2%, UV, IR, MS;
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Embodiment 2
Get Radix clausenae lansii skin 10Kg, 90% ethanol that adds 100L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 600W extracts each 10 minutes 3 times, combining extraction liquid, filter, decompression recycling ethanol also concentrates, and concentrating with ratio is that 5: 1 acetone-water mixed solvent carries out 6 stage countercurrents and extracts, the volume ratio of concentrated solution and the total consumption of mixed solvent is 1: 6, combining extraction liquid joins on the D102 type macroporous adsorptive resins and adsorbs 60% ethanol elution, collect 8 times of amount column volume elutriants, decompression recycling ethanol also concentrates, and adds the normal hexane crystallization, fractional crystallization, washing, be drying to obtain white platelet chalepensin 6.3g, detect through HPLC, purity is 94.8%, UV, IR, MS;
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Embodiment 3
Get Radix clausenae lansii skin 10Kg, 80% ethanol that adds 80L, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 500W extracts each 8 minutes 2 times, combining extraction liquid, filter, decompression recycling ethanol also concentrates, and concentrating with ratio is that 5: 1 acetone-water mixed solvent carries out 5 stage countercurrents and extracts, the volume ratio of concentrated solution and the total consumption of mixed solvent is 1: 5, combining extraction liquid joins on the AB8 type macroporous adsorptive resins and adsorbs 50% ethanol elution, collect 5 times of amount column volume elutriants, decompression recycling ethanol also concentrates, and adds the normal hexane crystallization, fractional crystallization, washing, be drying to obtain white platelet chalepensin 5.3g, detect through HPLC, purity is 98.3%, UV, IR, MS;
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Claims (8)
1. the preparation method of Yi Zhong chalepensin, it is characterized in that described method is made up of the following step: get the Radix clausenae lansii skin, add the 70-90% ethanol that its quality 6-10 doubly measures, drop in the microwave extracting apparatus and carry out microwave extracting, extraction power 300-600W, extract 1-3 time, each 3-10 minute, combining extraction liquid, filter, decompression recycling ethanol also concentrates, and concentrating with ratio is that 5: 1 acetone-water mixed solvent carries out the 3-6 stage countercurrent and extracts, and the volume ratio of concentrated solution and the total consumption of mixed solvent is 1: 3-6, combining extraction liquid, join on the macroporous adsorptive resins and adsorb, the 40-60% ethanol elution is collected 3-8 and is doubly measured the column volume elutriant, decompression recycling ethanol also concentrates, add the normal hexane crystallization, fractional crystallization, washing, be drying to obtain.
2. according to the preparation method of the described Yi Zhong of claim 1 chalepensin, it is characterized in that described microwave extracting concentration of ethanol is 80%, consumption is 8 times of amount volumes of raw materials quality.
3. according to the preparation method of the described Yi Zhong of claim 1 chalepensin, the power that it is characterized in that described microwave extracting is 500W.
4. according to the preparation method of the described Yi Zhong of claim 1 chalepensin, the number of times that it is characterized in that described microwave extracting is 2 times, each 8 minutes.
5. according to the preparation method of the described Yi Zhong of claim 1 chalepensin, the progression that it is characterized in that described counter-current extraction is 5 grades, and the volume ratio of concentrated solution and the total consumption of mixed solvent is 1: 5.
6. according to the preparation method of the described Yi Zhong of claim 1 chalepensin, it is characterized in that described macroporous adsorbent resin is selected from a kind of in D101 type, D102 type, the AB8 type macroporous adsorbent resin.
7. according to the preparation method of the described Yi Zhong of claim 1 chalepensin, it is characterized in that described macroporous adsorbent resin wash-out concentration of ethanol is 50%.
8. according to the preparation method of the described Yi Zhong of claim 1 chalepensin, it is characterized in that described macroporous adsorbent resin wash-out is 5 times of amount column volumes with the alcoholic acid collecting amount.
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| CN2010105541320A CN102030758A (en) | 2010-11-23 | 2010-11-23 | Preparation method of chalepensin |
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| CN2010105541320A CN102030758A (en) | 2010-11-23 | 2010-11-23 | Preparation method of chalepensin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329323A (en) * | 2011-05-31 | 2012-01-25 | 苏州派腾生物医药科技有限公司 | Method for extracting columbianadin from ligusticum daucoides franch |
| CN103285123A (en) * | 2013-06-20 | 2013-09-11 | 广东医学院 | Application of Chinese Wampee Fruit extract in drug-induced hepatitis control medicines |
| CN104383052B (en) * | 2014-12-01 | 2016-11-02 | 广东医学院 | Fructus clausenae lansii extract and in preparation for preventing and treating the application in Alzheimer disease drugs |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062069A (en) * | 2007-06-18 | 2007-10-31 | 石任兵 | Whole coumarins extract from root of dahuriae angelica and the preparing method thereof |
-
2010
- 2010-11-23 CN CN2010105541320A patent/CN102030758A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101062069A (en) * | 2007-06-18 | 2007-10-31 | 石任兵 | Whole coumarins extract from root of dahuriae angelica and the preparing method thereof |
Non-Patent Citations (2)
| Title |
|---|
| A.ULUBELEN: "a moskachan from ruta of chalepensis", 《PHYTOCHEMISTRY》 * |
| EZMIRLY,S.T.ET AL: "Saudi Arabian medicinal plants.I.Ruta chalepensis", 《J.CHEM.SOC.PAK.》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102329323A (en) * | 2011-05-31 | 2012-01-25 | 苏州派腾生物医药科技有限公司 | Method for extracting columbianadin from ligusticum daucoides franch |
| CN103285123A (en) * | 2013-06-20 | 2013-09-11 | 广东医学院 | Application of Chinese Wampee Fruit extract in drug-induced hepatitis control medicines |
| CN103285123B (en) * | 2013-06-20 | 2015-04-22 | 广东医学院 | Application of Chinese Wampee Fruit extract in drug-induced hepatitis control medicines |
| CN104383052B (en) * | 2014-12-01 | 2016-11-02 | 广东医学院 | Fructus clausenae lansii extract and in preparation for preventing and treating the application in Alzheimer disease drugs |
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Application publication date: 20110427 |