CN101216466B - Medlar HPLC fingerprint establishment method and its standard fingerprint - Google Patents
Medlar HPLC fingerprint establishment method and its standard fingerprint Download PDFInfo
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- CN101216466B CN101216466B CN2007103069386A CN200710306938A CN101216466B CN 101216466 B CN101216466 B CN 101216466B CN 2007103069386 A CN2007103069386 A CN 2007103069386A CN 200710306938 A CN200710306938 A CN 200710306938A CN 101216466 B CN101216466 B CN 101216466B
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Abstract
The invention provides a method for establishing an HPLC fingerprint spectrum of Fructus Lycii and a standard fingerprint spectrum thereof. The method comprises the following steps of: preparing a test solution, preparing a reference solution, selecting chromatographic conditions, and carrying out HPLC determination to obtain the fingerprint spectrum of Fructus Lycii. The standard fingerprint spectrum of Fructus Lycii can be obtained by comparing HPLC fingerprint spectra of 21 batches of Fructus Lycii materials and determining the common fingerprint characteristics. The method has the advantages of simple operation, good reproducibility, a plurality of characteristic peaks, accurate and reliable result, etc. The standard fingerprint spectrum can be used for effectively monitoring the quality of Fructus Lycii.
Description
Technical field
The present invention relates to a kind of method for building up of Chinese crude drug finger-print, the method for building up of matrimony vine medicinal material high performance liquid chromatography (HPLC) finger-print especially, and the resulting medlar HPLC standard finger-print of method thus.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 article 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 see from the angle of Chinese medicine total quality control, also reach the purpose that reflects effectively and control the total quality of Chinese medicine far away.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.
The fruit of Chinese wolfberry is the ripening fruits of matrimony vine of solanaceae plant, and another name FRUCTUS LYCII BARBARI, white thorn, mountain matrimony vine, white lump pin are called for short matrimony vine; Has tonifying kidney and benefiting sperm; Nourish the liver to improve visual acuity, blood-enriching tranquillizing promotes the production of body fluid to quench thirst; The effect that moistens the lung and relieve the cough clinically is mainly used in treatment liver-kidney Yin deficiency, soreness and weakness of waist and knees, has a dizzy spell, diseases such as the many tears of blurred vision and cough due to consumptive disease.Contain abundant LBP-X, fat, protein, free amino acid, taurine, betaine, vitamin B1, B2, E, C in the matrimony vine, in addition, also contain a large amount of mineral elements, like potassium, sodium, calcium, magnesium, iron, copper, manganese, zinc, selenium etc.At present, people also are only limited to the quality control of matrimony vine certain effective constituent in its many component or index property composition are carried out qualitative, quantitative test, lack the standard control device of reflection matrimony vine quality comprehensively.
Summary of the invention
The method for building up that the purpose of this invention is to provide a kind of medlar HPLC finger-print, and the resulting matrimony vine medicinal material of method standard finger-print thus.For realizing this purpose, the present invention has proposed a kind of matrimony vine quality of medicinal material control method through the research to the matrimony vine efficient liquid-phase chromatograph finger print atlas, has remedied the deficiency of existing Quality Control Technology, and the quality control of matrimony vine medicinal material is improved and science more.
The method for building up of medlar HPLC finger-print 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 100～800mL of 60～80%; Ultrasonic concussion 60min; Cooling back constant volume is got supernatant with 0.45 μ m filtering with microporous membrane, and filtrating 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 water-acetonitrile; Adopt the gradient elution mode: 0min → 15min → 30min → 45min → 60min, acetonitrile 10% → 22% → 35% → 45% → 55%; Flow velocity 0.8～1.2mL/min; Detect wavelength 254nm; 25～45 ℃ of column temperatures.Analyze need testing solution with this understanding, obtain the finger-print of matrimony vine medicinal material.
(3) confirming of standard finger-print: according to method provided by the invention; 21 batches of matrimony vine medicinal materials have been set up the HPLC finger-print; Through analyzing relatively; 13 common characteristic peaks have been confirmed; Its retention time is respectively: 2.4min, 3.9min, 5.4min, 10.8min, 14.0min, 19.7min, 24.1min, 28.5min, 29.2min, 38.9min, 43.3min, 47.0min, 59.8min, these common characteristic peaks have constituted the fingerprint characteristic of matrimony vine medicinal material, can be used as the standard finger-print of matrimony vine medicinal material.
The present invention has following significant advantage and purposes:
(1) the matrimony vine medicinal material is done as a whole treating, can find out the nuance between the different medicinal materials through comparing its total peak;
(2) test sample is simple for production, and chromatographic condition is realized easily;
(3) stability of method and reappearance are all relatively good;
(4) be suitable for discriminating and control to the matrimony vine medicinal material true and false, the place of production and quality.
Description of drawings
Fig. 1 is the standard finger-print of matrimony vine medicinal material provided by the invention.Its 13 common characteristic peaks have from left to right been marked respectively.
Embodiment
The preferred embodiments of the present invention are following:
(1) instrument and medicine: use Tianjin, island LC10A high performance liquid chromatograph; Totally 21 batches of matrimony vine 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 80% methyl alcohol 500mL, ultrasonic concussion 60min, cooling constant volume.Get supernatant with 0.45 μ m filtering with microporous membrane, filtrating 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 water-acetonitrile; Adopt the gradient elution mode: 0min → 15min → 30min → 45min → 60min, acetonitrile 10% → 22% → 35% → 45% → 55%; Flow velocity 1.0mL/min; Detect wavelength 254nm; 30 ℃ of column temperatures.Analyze need testing solution with this understanding, obtain the finger-print of matrimony vine medicinal material.
(4) according to method provided by the invention; 21 batches of matrimony vine medicinal materials have been set up the HPLC finger-print; Through analyzing relatively, confirmed 13 common characteristic peaks, its retention time is respectively: 2.4min, 3.9min, 5.4min, 10.8min, 14.0min, 19.7min, 24.1min, 28.5min, 29.2min, 38.9min, 43.3min, 47.0min, 59.8min; These common characteristic peaks have constituted the fingerprint characteristic of matrimony vine medicinal material, can be used as the standard finger-print of matrimony vine medicinal material.
Claims (1)
1. the method for building up of a matrimony vine medicinal material efficient liquid-phase chromatograph finger print atlas may further comprise the steps:
(1) preparation of need testing solution: precision takes by weighing matrimony vine medicinal powder 10g, places tool plug container, adds methyl alcohol 100～800mL of 60～80%; Ultrasonic concussion 60min; Cooling back constant volume is got supernatant with 0.45 μ m filtering with microporous membrane, and filtrating is as need testing solution;
(2) making of finger-print: the chromatographic resolution column packing is 5 μ m Kromasil-C18,250 * 4.6mm; Moving phase is water-acetonitrile; Adopt the gradient elution mode: 0min → 15min → 30min → 45min → 60min, acetonitrile 10% → 22% → 35% → 45% → 55%; Flow velocity 0.8～1.2mL/min; Detect wavelength 254nm; 25～45 ℃ of column temperatures; Analyze need testing solution with this understanding, obtain the finger-print of matrimony vine medicinal material;
(3) confirming of standard finger-print: confirmed 13 common characteristic peaks; Its retention time is respectively: 2.4min, 3.9min, 5.4min, 10.8min, 14.0min, 19.7min, 24.1min, 28.5min, 29.2min, 38.9min, 43.3min, 47.0min, 59.8min; These common characteristic peaks have constituted the fingerprint characteristic of matrimony vine medicinal material, can be used as the standard finger-print of matrimony vine medicinal material.
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| CN2007103069386A CN101216466B (en) | 2007-12-28 | 2007-12-28 | Medlar HPLC fingerprint establishment method and its standard fingerprint |
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| CN2007103069386A CN101216466B (en) | 2007-12-28 | 2007-12-28 | Medlar HPLC fingerprint establishment method and its standard fingerprint |
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| CN101216466B true CN101216466B (en) | 2012-01-04 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102749348B (en) * | 2012-06-18 | 2014-06-11 | 河南省科高植物天然产物开发工程技术有限公司 | Method for identifying active components in medicinal plant |
| CN103048347B (en) * | 2012-08-15 | 2014-06-11 | 河南省科高植物天然产物开发工程技术有限公司 | Method for distinguishing root-bark medicinal materials of celastrus angulatus |
| CN103630618A (en) * | 2013-04-02 | 2014-03-12 | 汕头市创美中药饮片有限公司 | Method for determining betaine content in wolfberry |
| CN104458985B (en) * | 2014-10-14 | 2016-04-06 | 中国药科大学 | The construction method of the polynary finger-print of LBP-X and standard finger-print thereof |
| CN111458447B (en) * | 2020-05-11 | 2023-03-31 | 贵州中医药大学 | Chinese wolfberry quality detection method based on spectral efficiency relationship |
| CN113109469B (en) * | 2021-03-29 | 2023-05-26 | 青海省食品检验检测院 | Detection method of wolfberry bud tea |
| CN113984916B (en) * | 2021-09-28 | 2024-04-19 | 天津中医药大学第一附属医院 | Method for measuring content of marrow-correcting pill and marrow-correcting pill medicine material |
| CN114487205B (en) * | 2022-02-15 | 2023-01-24 | 中国中医科学院中药研究所 | Construction method of fingerprint spectrum of Ningxia wolfberry |
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Non-Patent Citations (2)
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| 卢红梅等.枸杞的高效液相色谱指纹图谱.《中南大学学报（自然科学版）》.2005,第36卷(第2期),248-252. * |
| 张自萍等.宁夏枸杞高效液相色谱指纹图谱研究.《中成药》.2007,第29卷(第11期),1566-1570. * |
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