CN102771747B - Method for extracting tingling substance from zanthoxylum oil - Google Patents
Method for extracting tingling substance from zanthoxylum oil Download PDFInfo
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- CN102771747B CN102771747B CN201210289574.6A CN201210289574A CN102771747B CN 102771747 B CN102771747 B CN 102771747B CN 201210289574 A CN201210289574 A CN 201210289574A CN 102771747 B CN102771747 B CN 102771747B
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- essential oil
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- zanthoxylum essential
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Abstract
The invention relates to a method for extracting a tingling substance from zanthoxylum oil. The method comprises the following steps of: accurately weighing 0.1g zanthoxylum oil and putting into a volumetric flask of 10mL, using absolute methanol to reach a constant volume of a graduation, shaking up, leaching for 4 hours at 30 DEG C, cooling, then transferring into a centrifuging test tube with a graduation of 10mL, centrifuging, taking 0.1mL supernatant and putting into a volumetric flask of 10mL, using absolute methanol to reach a constant volume of a graduation, shaking up, filtering by a 0.2mu m filter membrane to obtain a liquid to be tested, performing semi-preparative high performance liquid chromatography separation on the liquid to be tested, collecting distillate by a distillate collector at a starting time of 9.0 minute and an end time of 11.6 minute, collecting effluent liquid of the distillate collector, after sampling for many times, combining the effluent liquid, and concentrating to remove the solvent to obtain the tingling substance of zanthoxylum oil. The method for preparing the tingling substance from zanthoxylum oil provided by the invention has simple operation steps and low equipment request.
Description
Technical field
The present invention relates to a kind of method extracting Zanthoxylum essential oil spicy components, particularly a kind of method utilizing semi-preparative reverse-phase high performance liquid chromatography to extract Zanthoxylum essential oil spicy components.
Background technology
Zanthoxylum essential oil refers to application supercritical CO
2the xanthoxylum oleoresin that the methods such as extraction, organic solvent extraction are extracted from Chinese prickly ash and the flavored oils with spicy hot taste that appropriate amount of edible oil is mixed, or directly soak the flavored oils with spicy hot taste made by Chinese prickly ash with edible oil.In Zanthoxylum essential oil, the power of numb taste directly affects its quality, and present Zanthoxylum essential oil spicy components, without commodity selling, need rely on self-control.The object of this invention is to provide a kind of method utilizing semi-preparative reverse-phase high performance liquid chromatography to extract Zanthoxylum essential oil spicy components.
Summary of the invention
The object of this invention is to provide a kind of method extracting Zanthoxylum essential oil spicy components, solve the problem without the merchandise sales of Zanthoxylum essential oil spicy components in prior art, obtained Zanthoxylum essential oil spicy components.
The technical solution used in the present invention is:
A kind of method extracting Zanthoxylum essential oil spicy components, the method comprises the steps: accurately to take 0.1g Zanthoxylum essential oil in 10mL volumetric flask, scale is settled to absolute methanol, shake up, lixiviate 4h at 30 DEG C, after cooling, proceed in 10mL scale centrifuge tube, centrifugal, get supernatant 0.1mL in 10mL volumetric flask, scale is settled to absolute methanol, shake up, liquid to be measured is after 0.2 μm of membrane filtration, liquid to be measured is carried out the separation of Semipreparative chromatography method, carry out fraction collection, the time started collected by fraction collector is 9.0min, end time is 11.6min, collect the efflux of fraction collector, repeatedly after sample introduction, merge efflux, concentrated removal solvent, obtain Zanthoxylum essential oil spicy components.
Preferably, the condition that described Semipreparative chromatography method is separated is:
Agilent 1200 type high performance liquid chromatograph (quaternary pump, online degasser, automatic sampler, column oven, DAD detector and ChemStation chromatographic work station),
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 × 150mm, 5 μm),
Mobile phase consists of methyl alcohol: water=60:40, flow velocity 1.0mL/min, column temperature 30 DEG C,
DAD scanning wavelength 254nm, reference wavelength 360nm, sample size 20 μ L.
The advantage that the present invention has and beneficial effect:
The present invention efficiently solves the problem of Zanthoxylum essential oil spicy components without commodity selling, provides a kind of method preparing Zanthoxylum essential oil spicy components, and operating procedure is simple, and equipment requirement is not high.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
Embodiment 1
Utilize semi-preparative reverse-phase high performance liquid chromatography to extract a method for Zanthoxylum essential oil spicy components, the method comprises the steps:
1), the extraction of Zanthoxylum essential oil spicy component
Accurately take 0.1g Zanthoxylum essential oil in 10mL volumetric flask, scale is settled to absolute methanol, shake up, lixiviate 4h at 30 DEG C, after cooling, proceed in 10mL scale centrifuge tube, centrifugal, get supernatant 0.1mL in 10mL volumetric flask, be settled to scale with absolute methanol, shake up, after 0.2 μm of membrane filtration, be liquid to be measured;
2), the chromatographiccondition of Zanthoxylum essential oil spicy component and fraction collection condition
Agilent 1200 type high performance liquid chromatograph (quaternary pump, online degasser, automatic sampler, column oven, DAD detector and ChemStation chromatographic work station) and fraction collector
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 × 150mm, 5 μm),
Mobile phase consists of methyl alcohol: water=60:40, flow velocity 1.0mL/min, column temperature 30 DEG C,
DAD scanning wavelength 254nm, reference wavelength 360nm, sample size 20 μ L,
The time started collected by fraction collector is 9.0min, and the end time is 11.6min.
Collect the efflux of fraction collector, repeatedly after sample introduction, merge efflux, concentrated removal solvent, obtains Zanthoxylum essential oil spicy components.
Claims (1)
1. one kind is extracted the method for Zanthoxylum essential oil spicy components, it is characterized in that: the method comprises the steps: accurately to take 0.1g Zanthoxylum essential oil in 10mL volumetric flask, scale is settled to absolute methanol, shake up, lixiviate 4h at 30 DEG C, after cooling, proceed in 10mL scale centrifuge tube, centrifugal, get supernatant 0.1mL in 10mL volumetric flask, scale is settled to absolute methanol, shake up, liquid to be measured is after 0.2 μm of membrane filtration, liquid to be measured is carried out the separation of Semipreparative chromatography method, carry out fraction collection, the time started collected by fraction collector is 9.0min, end time is 11.6min, collect the efflux of fraction collector, repeatedly after sample introduction, merge efflux, concentrated removal solvent, obtain Zanthoxylum essential oil spicy components,
The condition that described Semipreparative chromatography method is separated is:
Agilent 1200 type high performance liquid chromatograph;
Chromatographic column: ZORBAX Eclipse XDB-C18 (4.6 × 150mm, 5 μm);
Mobile phase consists of methyl alcohol: water=60:40, flow velocity 1.0mL/min, column temperature 30 DEG C;
DAD scanning wavelength 254nm, reference wavelength 360nm, sample size 20 μ L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210289574.6A CN102771747B (en) | 2012-08-14 | 2012-08-14 | Method for extracting tingling substance from zanthoxylum oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210289574.6A CN102771747B (en) | 2012-08-14 | 2012-08-14 | Method for extracting tingling substance from zanthoxylum oil |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102771747A CN102771747A (en) | 2012-11-14 |
| CN102771747B true CN102771747B (en) | 2015-06-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210289574.6A Active CN102771747B (en) | 2012-08-14 | 2012-08-14 | Method for extracting tingling substance from zanthoxylum oil |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113367308A (en) * | 2021-01-22 | 2021-09-10 | 中国标准化研究院 | Spicy material without spice, natural spicy essence and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000327567A (en) * | 1999-05-18 | 2000-11-28 | Susumu Kurosawa | Agent for improving movement of digestive canal |
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2012
- 2012-08-14 CN CN201210289574.6A patent/CN102771747B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000327567A (en) * | 1999-05-18 | 2000-11-28 | Susumu Kurosawa | Agent for improving movement of digestive canal |
Non-Patent Citations (2)
| Title |
|---|
| 付陈梅,等.紫外分光光度计法测花椒油中酞胺类物质含量.《中国食品添加剂》.2003,(第6期),第100-102页. * |
| 花椒麻味物质标准品的制备技术及其替代品的筛选与应用;孟一娟;《中国优秀硕士论文全文数据库工程科技1辑》;20100930(第9期);第11页 * |
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| CN102771747A (en) | 2012-11-14 |
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Effective date of registration: 20190306 Address after: No. 11 Libei Road, Dongli Economic Development Zone, Tianjin 300300 Patentee after: Tianjin Chunfa Biotechnology Group Co., Ltd. Address before: No. 30 Erwei Road, Dongli Economic Development Zone, Tianjin 300300 Patentee before: Tianjin Chunsheng Halal Foods Co., Ltd. |