CN102093243A - Method for preparing nordihydrocapsaicin - Google Patents
Method for preparing nordihydrocapsaicin Download PDFInfo
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- CN102093243A CN102093243A CN2010102971651A CN201010297165A CN102093243A CN 102093243 A CN102093243 A CN 102093243A CN 2010102971651 A CN2010102971651 A CN 2010102971651A CN 201010297165 A CN201010297165 A CN 201010297165A CN 102093243 A CN102093243 A CN 102093243A
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- dihydrocapsaicin
- extraction
- capsicum
- methyl alcohol
- capsicum resin
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Abstract
The invention relates to a method for preparing nordihydrocapsaicin, which comprises the following step: separating capsicum resin (also called capsicum oleoresin) by a semipreparative high-efficiency liquid chromatography. The nordihydrocapsaicin prepared by the method provided by the invention has high purity, thereby effectively solving the problem that the standard nordihydrocapsaicin substance can not be easily found in the market.
Description
Technical field
The present invention relates to a kind of preparation method who falls Dihydrocapsaicin, the method for Dihydrocapsaicin falls in the preparation of particularly a kind of use half preparative high performance liquid chromatography.
Background technology
Capsaicine class material is that the structure that is contained in the fruit of capsicum is the alkaloid monomer mixture of N-vanillyl amide, is the taste compound of capsicum.Contain more than ten kind of composition in the capsaicine class material, be mainly capsaicine, Dihydrocapsaicin, fall Dihydrocapsaicin etc.At present, the reference material of capsaicine and Dihydrocapsaicin can bought on the market, but falls difficult searching of reference material of Dihydrocapsaicin.
Summary of the invention
The objective of the invention is to seek, provide a kind of preparation to fall the method for Dihydrocapsaicin at the reference material that falls Dihydrocapsaicin is difficult.
Technical scheme of the present invention is:
The method of Dihydrocapsaicin falls in a kind of preparation, and this method steps comprises that using half preparative high performance liquid chromatography separates capsicum resin (claiming oleoresin capsicum again).
Particularly, the method of Dihydrocapsaicin falls in a kind of preparation, this method may further comprise the steps: in capsicum resin: the ratio of methyl alcohol=1～10mg: 1～20mL is dissolved in capsicum resin in the methyl alcohol, supersound extraction 5-30min, behind 0.2 μ m membrane filtration, carrying out half preparative high performance liquid chromatography separates, collect the effluent liquid of run tank, repeatedly behind the sample introduction, effluent liquid is carried out underpressure distillation steam methyl alcohol, the ethyl acetate extraction water utilizes Rotary Evaporators solvent evaporated ethyl acetate, obtains monomeric compound and falls Dihydrocapsaicin.
Preferably, the preparation method of described capsicum resin leaves standstill after-filtration for red chilly powder is carried out supersound extraction with ethanol, gets extraction liquid, obtains capsicum resin after extraction liquid is concentrated.
Described red chilly powder is the conventional products of market sale.
Preferably, the isolating condition of described half preparative high-performance liquid chromatographic method is:
Chromatographic column: the C18 reverse-phase chromatographic column, as Eclipse XDB-C18 chromatographic column (4.6 * 150mm, 5 μ m).
Moving phase: volume ratio is 65: 35 a water-methanol solution,
Eluent flow rate: 1.0ml/min,
Detect wavelength: 230nm,
30 ℃ of column temperatures,
Detector is a diode-array detector.
Preferably, it is 9.7min that described run tank is collected the time opening, and the concluding time is 10.4min.
The beneficial effect that the present invention had:
Adopt the inventive method, what make falls Dihydrocapsaicin purity height, effectively solves to fall the Dihydrocapsaicin standard substance on the market and blame the problem of looking for.
Embodiment
The present invention is further described below in conjunction with specific embodiment, but do not limit the present invention.
Embodiment 1
Commercially available red chilly powder is carried out supersound extraction with ethanol, leave standstill after-filtration, get extraction liquid, obtain capsicum resin after the gained extraction liquid concentrated, get capsicum resin 100mg, be dissolved in the 10mL methyl alcohol, supersound extraction 10min behind 0.2 μ m membrane filtration, carries out half preparative high performance liquid chromatography and separates, collect the effluent liquid of run tank, repeatedly behind the sample introduction, effluent liquid is carried out underpressure distillation steam methyl alcohol, the ethyl acetate extraction water, utilize Rotary Evaporators solvent evaporated ethyl acetate, obtain monomeric compound and fall Dihydrocapsaicin.
Instrument: Agilent 1200 type high performance liquid chromatographs, join diode-array detector and run tank.
Chromatographic condition: Eclipse XDB-C18 chromatographic column (4.6 * 150mm, 5 μ m), moving phase is water-methanol (volume ratio is 65: 35), flow velocity is 1.0mL/min, column temperature is 30 ℃, and the detection wavelength is 230nm, and sampling volume is 100 μ L, it is 9.7min that run tank is collected the time opening, and the concluding time is 10.4min.
Claims (5)
1. one kind prepares the method for falling Dihydrocapsaicin, it is characterized in that: this method steps comprises that using half preparative high performance liquid chromatography separates capsicum resin.
2. the method for Dihydrocapsaicin falls in a kind of preparation according to claim 1, it is characterized in that: this method may further comprise the steps: in capsicum resin: the ratio of methyl alcohol=1～10mg: 1～20mL is dissolved in capsicum resin in the methyl alcohol, supersound extraction 5-30min, behind 0.2 μ m membrane filtration, carrying out half preparative high performance liquid chromatography separates, collect the effluent liquid of run tank, repeatedly behind the sample introduction, effluent liquid is carried out underpressure distillation steam methyl alcohol, the ethyl acetate extraction water, utilize Rotary Evaporators solvent evaporated ethyl acetate, obtain monomeric compound and fall Dihydrocapsaicin.
3. the method for Dihydrocapsaicin falls in a kind of preparation according to claim 2, it is characterized in that: the preparation method of described capsicum resin is for to carry out supersound extraction with red chilly powder with ethanol, leave standstill after-filtration, get extraction liquid, obtain capsicum resin after extraction liquid is concentrated.
4. fall the method for Dihydrocapsaicin according to claim 2 or 3 described a kind of preparations, it is characterized in that: the isolating condition of described half preparative high-performance liquid chromatographic method is:
Chromatographic column: the C18 reverse-phase chromatographic column,
Moving phase: volume ratio is 65: 35 a water-methanol solution,
Eluent flow rate: 1.0ml/min,
Detect wavelength: 230nm,
30 ℃ of column temperatures,
Detector is a diode-array detector.
5. fall the method for Dihydrocapsaicin according to claim 2 or 3 described a kind of preparations, it is characterized in that: it is 9.7min that described run tank is collected the time opening, and the concluding time is 10.4min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102971651A CN102093243A (en) | 2010-09-29 | 2010-09-29 | Method for preparing nordihydrocapsaicin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010102971651A CN102093243A (en) | 2010-09-29 | 2010-09-29 | Method for preparing nordihydrocapsaicin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102093243A true CN102093243A (en) | 2011-06-15 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010102971651A Pending CN102093243A (en) | 2010-09-29 | 2010-09-29 | Method for preparing nordihydrocapsaicin |
Country Status (1)
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| CN (1) | CN102093243A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807770A (en) * | 2012-07-30 | 2012-12-05 | 江苏科技大学 | Method for preparing paprika red pigment by ultrasonic pre-treatment |
| CN108627373A (en) * | 2018-04-20 | 2018-10-09 | 三明出入境检验检疫局综合技术服务中心 | A kind of preparation method and application of chafing dish food matrix papaverine standard substance |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009115840A1 (en) * | 2008-03-18 | 2009-09-24 | Isis Innovation Limited | Method of electrochemically detecting a capsaicinoid in a sample |
| CN101619028A (en) * | 2009-06-17 | 2010-01-06 | 张鹏 | Method for preparing capsicine monomer |
-
2010
- 2010-09-29 CN CN2010102971651A patent/CN102093243A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009115840A1 (en) * | 2008-03-18 | 2009-09-24 | Isis Innovation Limited | Method of electrochemically detecting a capsaicinoid in a sample |
| CN101619028A (en) * | 2009-06-17 | 2010-01-06 | 张鹏 | Method for preparing capsicine monomer |
Non-Patent Citations (1)
| Title |
|---|
| 董新荣等: "制备型高效液相色谱法制备纯化3种辣椒素单体", 《色谱》, vol. 26, no. 03, 30 May 2008 (2008-05-30), pages 366 - 369 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807770A (en) * | 2012-07-30 | 2012-12-05 | 江苏科技大学 | Method for preparing paprika red pigment by ultrasonic pre-treatment |
| CN108627373A (en) * | 2018-04-20 | 2018-10-09 | 三明出入境检验检疫局综合技术服务中心 | A kind of preparation method and application of chafing dish food matrix papaverine standard substance |
| CN108627373B (en) * | 2018-04-20 | 2021-11-09 | 三明出入境检验检疫局综合技术服务中心 | Preparation method and application of papaverine standard substance serving as hot pot food matrix |
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Application publication date: 20110615 |