CN101183092A - Construction method of globeflower medicinal materials fingerprint and standard fingerprint thereof - Google Patents
Construction method of globeflower medicinal materials fingerprint and standard fingerprint thereof Download PDFInfo
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- CN101183092A CN101183092A CN 200710306936 CN200710306936A CN101183092A CN 101183092 A CN101183092 A CN 101183092A CN 200710306936 CN200710306936 CN 200710306936 CN 200710306936 A CN200710306936 A CN 200710306936A CN 101183092 A CN101183092 A CN 101183092A
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Abstract
The present invention provides a construction method of a golden lotus medicinal material fingerprint and a standard fingerprint. The proper amount of methanol is added into golden lotus medicinal material powder; the mixture is soaked for 24 hours and extracted by ultrasound for 30 minutes; and then the clear liquid is filtered through a microporous membrane; and the filtrate is sample solution; high performance liquid chromatographic analysis sample solution is carried out to the sample solution; the chromatographic column is Kromasil-C18 (5 Mu m, 250*4.6mm), the temperature of the column is 40 DEG C. Mobile phrase is methanol-water; a gradient elution method is applied; detecting wavelength is 350 nm; and then the HPLC fingerprint of the golden lotus medicinal material is gained. Fingerprint feature in common are ensured and the standard fingerprint is gained through comparing 14th batch golden lotus medicinal material fingerprint HPLC. The quality of the golden lotus medicinal material can be effectively controlled by using the standard fingerprint.
Description
Technical field
The present invention relates to the construction method of Chinese crude drug finger-print, especially the construction method and the standard finger-print thereof of globeflower medicinal materials high performance liquid chromatography (HPLC) finger-print.Belong to the Pharmaceutical Analysis technical field.
Background technology
Traditional Chinese medicine fingerprint refers in particular to the collection of illustrative plates or the image of each component population characteristic of Chinese medicine that the Chinese medicine sample obtains through modern analytical techniques such as spectrum or chromatograms.At present finger-print has become the discriminating herbal species of generally acknowledging both at home and abroad and has estimated one of effective means of traditional Chinese medicine quality.FDA (Food and Drug Adminstration) is in " FDA is about the guide of vegetable products " formulated in 1996, and requiring provides corresponding finger-print to product and autonomic drug product in the middle of plant material, the autonomic drug.Medicinal and the fragrant plant association of British Herbal Pharmacopoeia, India herbal medicine allusion quotation and Canada, German medicinal plant association also accept chromatographic fingerprinting.China national drug regulatory department has issued " technical requirement (provisional) of the finger-print research of traditional Chinese medicine " in 2000, explicitly call for traditional Chinese medicine of newly declaring and the traditional Chinese medicine that has gone on the market are carried out the finger-print standard.
Traditional Chinese medicine fingerprint has passed through the research of many decades, many modern analysis means of testing such as comprising ultraviolet, infrared, gas phase, high performance liquid chromatogram, thin layer, nuclear magnetic resonance, scanning electron microscope, computer image analysis, electrophoretic techniques, isoenzyme analysis method, Protocols in Molecular Biology, cluster analysis technology have been used, for the material of Chinese medicine is identified and constituent analysis has accumulated lot of data.But, also reach the purpose that reflects effectively and control the total quality of Chinese medicine far away from the angle of Chinese medicine total quality control.High performance liquid chromatography (HPLC) finger-print obtains approval in the world easily, comprises that many countries of the U.S., Britain, France, Canada, Germany, Japan and India more are ready to accept the HPLC finger-print.Therefore, setting up corresponding HPLC finger-print for Chinese crude drug, is the effective means of present stage control Chinese medicine inherent quality.
Trollflower is the dried floral of ranunculaceae plant trollflower, is distributed widely in China northeast, North China and area, the Inner Mongol.Trollflower has antibacterial and clearing heat and detoxicating effect, is usually used in acute and chronic tonsillitis, otitis media acuta, acute myringitis, acute conjunctivitis, acute lymphangitis.Bibliographical information is many to the research of globeflower medicinal materials to be quantitative target with the general flavone, but under the situation that big portion active component it be unclear that, the amount of measuring one or two chemical constitution can't really reflect the crude drug quality of stability.
Summary of the invention
The construction method that the purpose of this invention is to provide a kind of globeflower medicinal materials fingerprint, and the resulting globeflower medicinal materials standard finger-print of method thus.For realizing this purpose, the present invention is by the research to the globeflower medicinal materials efficient liquid-phase chromatograph finger print atlas, proposed a kind of method of quality control of globeflower medicinal materials preferably, remedied the deficiency of existing Quality Control Technology, the quality control of globeflower medicinal materials is improved and science more.
The construction method of globeflower medicinal materials efficient liquid-phase chromatograph finger print atlas of the present invention comprises the steps:
(1) preparation of need testing solution: precision takes by weighing medicinal powder 10g, places tool plug container, adds methyl alcohol 100～700mL of 60～100%, soak 24h, ultrasonic concussion 30min, cooling back constant volume, get supernatant with 0.45 μ m filtering with microporous membrane, filtrate is as need testing solution.
(2) efficient liquid phase chromatographic analysis: the chromatographic resolution column packing is 5 μ m Kromasil-C18,250 * 4.6mm; Moving phase is methanol-water; Adopt the gradient elution mode: 0min → 25min → 60min → 85min → 120min, methyl alcohol 10% → 18% → 25% → 38% → 50%; Flow velocity 0.8～1.2mL/min; Detect wavelength 350nm; 30～45 ℃ of column temperatures.Analyze need testing solution with this understanding, obtain the finger-print of globeflower medicinal materials.
According to method provided by the invention, 14 batches of globeflower medicinal materials have been set up the HPLC finger-print, by analyzing relatively, 17 common characteristic peaks have been determined, its retention time is respectively: 4.8min, 7.7min, 10.9min, 17.6min, 28.0min, 33.5min, 41.3min, 43.8min, 48.0min, 53.2min, 57.1min, 62.3min, 82.7min, 86.2min, 94.0min, 101.1min, 109.5min, these common characteristic peaks have constituted the fingerprint characteristic of globeflower medicinal materials, can be used as the standard finger-print of globeflower medicinal materials.
The present invention does as a whole treating with globeflower medicinal materials, can find out nuance between the different medicinal materials by its total peak relatively, is suitable for discriminating and control to the globeflower medicinal materials true and false, the place of production and quality.
Description of drawings
Fig. 1 is the standard finger-print of globeflower medicinal materials provided by the invention.From left to right marked No. 1 to 17, its common characteristic peak among the figure respectively.
Embodiment
The preferred embodiments of the present invention are as follows:
(1) instrument and medicine: use Tianjin, island LC10A high performance liquid chromatograph; Totally 14 batches of globeflower medicinal materials are all purchased in the Chinese herbal medicine shop; Other reagent is chromatographically pure or analyzes pure.
(2) preparation of need testing solution: precision takes by weighing medicinal powder 10g, places volumetric flask, adds 75% methyl alcohol 400mL, soaks 24h, ultrasonic concussion 30min, and cooling back constant volume is got supernatant with 0.45 μ m filtering with microporous membrane, and filtrate is as need testing solution.
(3) efficient liquid phase chromatographic analysis: the chromatographic resolution column packing is 5 μ m Kromasil-C18,250 * 4.6mm; Moving phase is methanol-water; Adopt the gradient elution mode: 0min → 25min → 60min → 85min → 120min, methyl alcohol 10% → 18% → 25% → 38% → 50%; Flow velocity 1.0mL/min; Detect wavelength 350nm; 40 ℃ of column temperatures.Analyze need testing solution with this understanding, obtain the finger-print of globeflower medicinal materials.
(4) according to method provided by the invention, 14 batches of globeflower medicinal materials have been set up the HPLC finger-print, 17 common characteristic peaks have been determined, its retention time is respectively: 4.8min, 7.7min, 10.9min, 17.6min, 28.0min, 33.5min, 41.3min, 43.8min, 48.0min, 53.2min, 57.1min, 62.3min, 82.7min, 86.2min, 94.0min, 101.1min, 109.5min, these common characteristic peaks have constituted the fingerprint characteristic of globeflower medicinal materials, can be used as the standard finger-print of globeflower medicinal materials.
Claims (4)
1. the method for building up of a globeflower medicinal materials efficient liquid-phase chromatograph finger print atlas, its feature comprise preparation, the making of finger-print and the determining of standard finger-print of need testing solution.
2. the method for building up of globeflower medicinal materials efficient liquid-phase chromatograph finger print atlas according to claim 1, the preparation method who it is characterized in that described need testing solution is: precision takes by weighing medicinal powder 10g, place tool plug container, methyl alcohol 100～the 700mL of adding 60～100%, soak 24h, ultrasonic concussion 30min, cooling back constant volume, get supernatant with 0.45 μ m filtering with microporous membrane, filtrate is as need testing solution.
3. according to the method for building up of claim 1,2 described globeflower medicinal materials efficient liquid-phase chromatograph finger print atlas, it is characterized in that the manufacturing process of described finger-print is: the chromatographic resolution column packing is 5 μ m Kromasil-C18,250 * 4.6mm; Moving phase is methanol-water; Adopt the gradient elution mode: 0min → 25min → 60min → 85min → 120min, methyl alcohol 10% → 18% → 25% → 38% → 50%; Flow velocity 0.8～1.2mL/min; Detect wavelength 350nm; 30～45 ℃ of column temperatures.Analyze need testing solution with this understanding, obtain the finger-print of globeflower medicinal materials.
4. according to claim 1,2, the method for building up of 3 described globeflower medicinal materials efficient liquid-phase chromatograph finger print atlas, the definite method that it is characterized in that described standard finger-print is: according to method provided by the invention, 14 batches of globeflower medicinal materials have been set up the HPLC finger-print, by analyzing relatively, 17 common characteristic peaks have been determined, its retention time is respectively: 4.8min, 7.7min, 10.9min, 17.6min, 28.0min, 33.5min, 41.3min, 43.8min, 48.0min, 53.2min, 57.1min, 62.3min, 82.7min, 86.2min, 94.0min, 101.1min, 109.5min, these common characteristic peaks have constituted the fingerprint characteristic of globeflower medicinal materials, can be used as the standard finger-print of globeflower medicinal materials.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2007103069367A CN101183092B (en) | 2007-12-28 | 2007-12-28 | Construction method of globeflower medicinal materials fingerprint and standard fingerprint thereof |
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| CN2007103069367A CN101183092B (en) | 2007-12-28 | 2007-12-28 | Construction method of globeflower medicinal materials fingerprint and standard fingerprint thereof |
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| CN101183092A true CN101183092A (en) | 2008-05-21 |
| CN101183092B CN101183092B (en) | 2011-05-11 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103245739A (en) * | 2013-04-08 | 2013-08-14 | 江苏康缘药业股份有限公司 | Method for determining fingerprint of fructus forsythia detoxication soft capsule |
| CN104458632A (en) * | 2014-11-27 | 2015-03-25 | 山东大学 | Method for detecting and distinguishing traditional Chinese medicines with same quality |
| CN106706835A (en) * | 2016-11-28 | 2017-05-24 | 广东大鹏医药科技有限公司 | Quality detection method of trollius chinensis bunge effervescent tablets |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1996008A (en) * | 2006-11-02 | 2007-07-11 | 宁夏启元药业有限公司 | Identification method for Chinese globe flower and amygdalin in Chinese globe flower antipyretic capsule |
-
2007
- 2007-12-28 CN CN2007103069367A patent/CN101183092B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103245739A (en) * | 2013-04-08 | 2013-08-14 | 江苏康缘药业股份有限公司 | Method for determining fingerprint of fructus forsythia detoxication soft capsule |
| CN104458632A (en) * | 2014-11-27 | 2015-03-25 | 山东大学 | Method for detecting and distinguishing traditional Chinese medicines with same quality |
| CN106706835A (en) * | 2016-11-28 | 2017-05-24 | 广东大鹏医药科技有限公司 | Quality detection method of trollius chinensis bunge effervescent tablets |
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| CN101183092B (en) | 2011-05-11 |
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Granted publication date: 20110511 Termination date: 20121228 |