CN108490095A - A kind of method of Multiple components assay in pilose gerbera herb medicinal material - Google Patents

A kind of method of Multiple components assay in pilose gerbera herb medicinal material Download PDF

Info

Publication number
CN108490095A
CN108490095A CN201810313063.0A CN201810313063A CN108490095A CN 108490095 A CN108490095 A CN 108490095A CN 201810313063 A CN201810313063 A CN 201810313063A CN 108490095 A CN108490095 A CN 108490095A
Authority
CN
China
Prior art keywords
pilose gerbera
gerbera herb
medicinal material
acid
herb medicinal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201810313063.0A
Other languages
Chinese (zh)
Other versions
CN108490095B (en
Inventor
刘春花
孙佳
陆苑
潘洁
李勇军
马雪
李月婷
陈思颖
王爱民
王永林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Guizhou Medical University
Original Assignee
Guizhou Medical University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Guizhou Medical University filed Critical Guizhou Medical University
Priority to CN201810313063.0A priority Critical patent/CN108490095B/en
Publication of CN108490095A publication Critical patent/CN108490095A/en
Application granted granted Critical
Publication of CN108490095B publication Critical patent/CN108490095B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Medicinal Preparation (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to Chinese medicine detection technique field, the method for Multiple components assay in specifically a kind of pilose gerbera herb medicinal material.The present invention uses UPLC PDA methods, with Waters BET C18(2.1 × 150mm, 1.7 μm) is chromatographic column, and 0.1% aqueous formic acid of acetonitrile carries out gradient elution, and Detection wavelength is 280nm and 328nm, flow velocity 0.28mL/min, 40 DEG C of column temperature.The method according to the invention, pilose gerbera herb medicinal material Content of Chlorogenic Acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, galuteolin and ursin are preferably detached, and the sample recovery rate of method is 97.20% 103.57%, RSD≤3.0%.This method is easy, accurate, reproducible, can be used for the assay of pilose gerbera herb medicinal material Content of Chlorogenic Acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, galuteolin and ursin, reference frame is provided for the quality control of pilose gerbera herb.

Description

A kind of method of Multiple components assay in pilose gerbera herb medicinal material
Technical field
The present invention relates to Chinese medicine detection technique field, Multiple components assay in specifically a kind of pilose gerbera herb medicinal material Method.
Background technology
Pilose gerbera herb is the dry of feverfew pilose gerbera herb Piloselloides hirsuta (Forsk.) G.Jeffrey Dry herb is also Minority Nationalities in Guizhou medication, be named as in Miao Minority " add eight old (the jab bat of Gong nexjongxjud)”.It is the mild-natured bitter of pilose gerbera herb, pungent, it attaches to the lung and stomach meridians, there is ventilating the lung and relieving cough, sweating Li Shui, the promoting flow of qi and blood circulation Effect is mainly used for cough due to common cold, asthma, oedema turgor, difficult urination, infantile indigestion with food retention, Amenorrhea, injury from falling down, carbuncle furuncle, furunculosis Etc. diseases.According to《The civil medicinal herbs in Kweiyang》It records, the cough of pilose gerbera herb primary treatment wind, cough, asthma and lung carbuncle etc. are relevant with lung Disease.Modern pharmacology research show pilose gerbera herb have the function of it is relieving cough and reducing sputum, relieving asthma.
Be currently known in pilose gerbera herb containing chlorogenic acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, galuteolin and A variety of phenolic acid class such as ursin and flavones ingredient, research shows that these ingredients may be its active constituent.Pilose gerbera herb quilt It records in version in 2003《Guizhou Province's Chinese medicine, Ethnic crude drugs quality standard》, 2005 years versions《Yunnan Province's The Quality of Sliced Herbal Medicine mark It is accurate》Etc. quality standards, but the content of wherein each beneficiating ingredient is not measured, pilose gerbera herb quality of medicinal material standard is endless at present It is kind, it cannot more comprehensively control the inherent quality of pilose gerbera herb medicinal material.
Therefore, pilose gerbera herb medicinal material Content of Chlorogenic Acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, different can be measured simultaneously by finding one kind The assay method of the multiple beneficials component content such as chlorogenic acid C, galuteolin and ursin, is the task of top priority.
Invention content
In order to solve the above technical problems existing in the prior art, a variety of in a kind of pilose gerbera herb medicinal material of present invention offer Component content method for measuring, includes the following steps:
A kind of method of Multiple components assay in pilose gerbera herb medicinal material, for measuring green original in pilose gerbera herb simultaneously The content of acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, galuteolin and ursin, which is characterized in that use UPLC- PDA methods are measured, with WatersBETC18(2.1 × 150mm, 1.7 μm) is chromatographic column, -0.1% aqueous formic acid of acetonitrile Gradient elution is carried out, while utilizing Detection wavelength 280nm and 328nm, flow velocity 0.28mL/min, 40 DEG C of column temperature.
The UPLC-PDA methods are used as test solution after diluting pilose gerbera herb herbal extract.
The pilose gerbera herb herbal extract is to extract to obtain to pilose gerbera herb medicinal material using methanol as solvent.Methanol pole Property is bigger than ethyl alcohol, and to effective component extracting, recovery rate is higher than ethyl alcohol, and acquired results are more acurrate.
It is described that pilose gerbera herb medicinal material is extracted using methanol as solvent, it is to be carried out to pilose gerbera herb medicinal material with 50% methanol Refluxing extraction, reflux extracting time 2h.Extraction efficiency is higher at this time, and will not lead to the beneficiating ingredient in pilose gerbera herb medicinal material It is destroyed.
The dilution is that pilose gerbera herb herbal extract is diluted 5 times with distilled water.UPLC-PDA is surveyed after this dilution proportion It is preferable to determine effect.
The pilose gerbera herb medicinal material was the pilose gerbera herb medicinal powder of No. three sieves.Cross the pilose gerbera herb medicinal material of No. three sieves Powder extraction effect is preferable.
Preferably, the UPLC-PDA methods, wherein test solution are prepared via a method which:Took No. three sieves Pilose gerbera herb medicinal powder 0.5g, and it is accurately weighed, set in conical flask with cover, 50% methanol 25mL is added in precision, weighed heavy Amount, is heated to reflux 2 hours, lets cool, then weighed weight, the weight of less loss is supplied with 50% methanol, is shaken up, and filters, and measures continuous filter Liquid 5ml, is transferred in 25ml volumetric flasks, is diluted to scale with distilled water, shakes up to get test solution.Pilose gerbera herb at this time Medicinal material extract is more efficient, and test liquid concentration is also relatively mild, and it is more accurate to measure acquired results.
The concrete operation step of the present invention is as follows:
(1) reference substance solution and test solution are prepared;
The preparation of reference substance solution:Precision weighs chlorogenic acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, wood respectively Rhinoceros grass glycosides and ursin are placed in right amount in 10mL measuring bottles, are added methanol to dissolve and are settled to scale, are obtained chlorogenic acid concentration respectively and are A concentration of 0.987mg/mL of 1.80mg/mL, 3,5-Dicaffeoylquinic acid, a concentration of 0.963mg/mL of 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid are a concentration of The reference substance storing solution of a concentration of 0.991mg/mL of 0.963mg/mL, galuteolin and a concentration of 1.92mg/mL of ursin.Respectively Precision measures above-mentioned 6 kinds of reference substance storing solutions through diluting in the same 10mL volumetric flasks of postposition, adds 50% methanol dilution to scale, It shakes up, obtains mixed reference substance solution, chlorogenic acid concentration is 9.00 μ g/mL, a concentration of 24.7 μ g/mL of 3,5-Dicaffeoylquinic acid, isochlorogenic acid A concentration of 9.63 μ g/mL of B, a concentration of 9.63 μ g/mL of 4,5-Dicaffeoylquinic acid, a concentration of 9.91 μ g/mL of galuteolin and ursin concentration For 3.84 μ g/mL, saved backup in 4 DEG C.
The preparation of test solution:Pilose gerbera herb medicinal powder (crossing No. three sieves) about 0.5g is taken, it is accurately weighed, set tool plug cone In shape bottle, 50% methanol 25mL is added in precision, and weighed weight is heated to reflux 2 hours, lets cool, then weighed weight, with 50% methanol The weight for supplying less loss, shakes up, and filtration measures in subsequent filtrate 5ml to 25ml volumetric flasks, is diluted to scale with distilled water, shakes up, Up to test solution.
(2) continuous mode:Mixed reference substance solution and test solution are taken respectively, is measured using UPLC-PDA, and chromatography is obtained Figure, ursin measure at a wavelength of 280 nm, remaining 5 kinds of compound measures under 328nm, and 6 ingredients and other substance peaks are complete It is fully separating.Wherein chromatographic condition is:Chromatographic column is WatersBETC18(2.1 × 150mm, 1.7 μm), mobile phase are acetonitrile- 0.1% aqueous formic acid carries out gradient elution, Detection wavelength 280nm and 328nm, flow velocity 0.28mL/min, 40 DEG C of column temperature, into 10 μ L of sample amount.
Step 3:Linear relationship investigation, Precision Experiment, repetitive test, stability test and sample-adding recycling are carried out respectively Rate is tested.
Sample preparation methods screen:
In order to select stable sample preparation methods, using solvent, extracting mode, extraction time as variable, to pilose gerbera herb Extracting method carry out screening test, it is as a result as follows:
From upper data:When using 50% methanol as solvent, extraction efficiency is few compared with high and impurity;Ultrasonic extraction and water-bath are returned Stream extraction is compared, and refluxing extraction efficiency is higher;The extraction effect of reflux 1h is poor, and the extraction effect for the 2h and 3h that flows back is without larger difference It is different.
Measure wavelength screening:
Since the ingredient to be measured of these in pilose gerbera herb has UV absorption, thus selection UV detector to ingredient to be measured into Row detection.
Full wavelength scanner is carried out through PDA detectors, the maximum absorption wavelength of each ingredient is as follows:
Ingredient Maximum absorption wavelength (nm)
Ursin 194.9、221.1、280.0
Chlorogenic acid 326.1
Luteolin 347.9
3,4-Dicaffeoylquinic acid 328.0
3,5-Dicaffeoylquinic acid 327.4
4,5-Dicaffeoylquinic acid 328.6
It is simultaneous by upper data it is found that the maximum absorption wavelength of ursin differs larger with the maximum absorption wavelength of other compositions It cares for and is detected in Same Wavelength, detection sensitivity can be significantly affected, considered, Double wavelength (280nm and 328nm) opposite 6 Kind ingredient carries out assay, measures ursin under 280nm, remaining 5 ingredient is surveyed under the conditions of 328nm, reaches same chromatostrip Part measures the purpose of different types of a variety of chemical compositions simultaneously.
In order to select suitable chromatographic condition, investigated different chromatographic columns, different flow phase systems, different mobile phase PH, Different mobile phase gradients, carry out multiple repetition test, and final choice is using 0.1% aqueous formic acid and acetonitrile as flowing Phase carries out gradient elution, final ursin, chlorogenic acid, galuteolin, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid and 4,5-Dicaffeoylquinic acid etc. 6 A ingredient is preferably detached.
This experiment is using the method for HPLC-PAD to 6 kinds of chemical composition ursin, chlorogenic acids, resedas in pilose gerbera herb Glycosides, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid and 4,5-Dicaffeoylquinic acid carry out assay, and this method processing is easy, has reached same chromatostrip Good separation has been carried out to 6 kinds of ingredients under part, it is linear good through methodology validation, repeatability, precision, stability and time Yield is preferable, can be used for pilose gerbera herb quality control.It analyzes, finds by being measured result to more batches of pilose gerbera herbs 6 kinds of component content fluctuations are larger, it is therefore desirable to the quality of pilose gerbera herb is controlled by multi objective.
Compared with prior art, the technique effect of the invention is embodied in:
The present invention uses UPLC-PDA methods, with Waters BET C18(2.1 × 150mm, 1.7 μm) is chromatographic column, - 0.1% aqueous formic acid of acetonitrile carries out gradient elution, and Detection wavelength is 280nm and 328nm, flow velocity 0.28mL/min, column temperature 40℃.The method according to the invention, pilose gerbera herb medicinal material Content of Chlorogenic Acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, sweet-scented osmanthus Careless glycosides and ursin are preferably detached, and the sample recovery rate of method is 97.20%-103.57%, RSD≤3.0%.The party Method is easy, accurate, reproducible, can be used for pilose gerbera herb medicinal material Content of Chlorogenic Acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, isochlorogenic acid C, the assay of galuteolin and ursin provides reference frame for the quality control of pilose gerbera herb.
Description of the drawings
Fig. 1 is system suitability experiment UPLC figures.
Wherein each absorption peak correspondence is as follows:1- ursin;2- chlorogenic acids;3- galuteolins;4- 3,4-Dicaffeoylquinic acids;5- 3,5-Dicaffeoylquinic acid;6- 4,5-Dicaffeoylquinic acids.
Specific implementation mode
It is limited with reference to specific embodiment technical scheme of the present invention is further, but claimed Range describes made by being not only limited to.
Embodiment:
Instrument and material:
Acquity UPLC-PDA systems (Waters companies, including binary super-pressure gradient pump, autosampler, chromatography Column oven, array two level pipe detector, Empower work stations);EL204 a ten thousandths electronic balance (plum Teller-support benefit instrument Device Shanghai Co., Ltd);Ultrapure water machine (Sichuan Water Technology Development Co., Ltd.);II type electric-heated thermostatic water baths of DK-98- (Tianjin Stettlen Instrument Ltd.).
Ursin reference substance (lot number:111951-201301), chlorogenic acid (lot number:And galuteolin (lot number 110753): 111720-201609) buy in National Institute for Food and Drugs Control;3,5-Dicaffeoylquinic acid (lot number:MUST-16031611), different Chlorogenic acid B (lot numbers:) and 4,5-Dicaffeoylquinic acid (lot number MUST-16031612:MUST-16031613) purchase is in Chengdu Man Sitesheng Object Science and Technology Ltd./Chengdu Inst. of Biology, Chinese Academy of Sciences.
Methanol (analysis is pure), ethyl alcohol (analysis is pure), acetonitrile (chromatographically pure) are bought in the limited public affairs of Chinese medicines group chemical reagent Department;Formic acid (chromatographically pure) is purchased from TEDIA Co., Ltds of the U.S..Experiment is with pilose gerbera herb medicinal material by Guizhou pharmaceutical college of medical university Crude drug is accredited as pilose gerbera herb Piloselloides hirsuta (Forsk.) with medicinal botany teaching and research room associate professor Zhang Xu The drying herb of G.Jeffrey.
It is prepared by contrast solution:
Precision weighs chlorogenic acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, galuteolin and appropriate ursin respectively It is placed in 10mL measuring bottles, methanol is added to dissolve and is settled to scale, it is dense for 1.80mg/mL, 3,5-Dicaffeoylquinic acid to obtain chlorogenic acid concentration respectively Degree is 0.987mg/mL, a concentration of 0.963mg/mL of 3,4-Dicaffeoylquinic acid, a concentration of 0.963mg/mL of 4,5-Dicaffeoylquinic acid, galuteolin are dense Degree is the reference substance storing solution of 0.991mg/mL and a concentration of 1.92mg/mL of ursin.It is accurate respectively to measure above-mentioned 6 kinds of reference substances Storing solution adds 50% methanol dilution to scale, shakes up, it is molten must to mix reference substance through diluting in the same 10mL volumetric flasks of postposition Liquid, chlorogenic acid concentration is 9.00 μ g/mL, a concentration of 24.7 μ g/mL of 3,5-Dicaffeoylquinic acid, a concentration of 9.63 μ g/mL of 3,4-Dicaffeoylquinic acid, different A concentration of 9.63 μ g/mL of chlorogenic acid C, a concentration of 9.91 μ g/mL of galuteolin and a concentration of 3.84 μ g/mL of ursin, in 4 DEG C of guarantors It deposits spare.
It is prepared by test solution:
Pilose gerbera herb is taken to cross the medicinal powder about 0.5g of No. three sieves, it is accurately weighed, it sets in conical flask with cover, precision is added 50% methanol 25mL, weighed weight are heated to reflux 2 hours, let cool, then weighed weight, and the weight of less loss is supplied with 50% methanol, It shakes up, filters, measure in subsequent filtrate 5ml to 25ml volumetric flasks, be diluted to scale with distilled water, shake up, filtered with 0.22 μm of micropore Membrane filtration takes subsequent filtrate as test solution, you can sample introduction is analyzed.
Chromatographic condition:
Chromatographic column is Waters BET C18(2.1 × 150mm, 1.7 μm), mobile phase are that acetonitrile (A) -0.1% formic acid is water-soluble Liquid (B) carries out gradient elution, Detection wavelength 280nm and 328nm, flow velocity 0.28mL/min, 40 DEG C of column temperature, 10 μ L of sample size, Elution program is as shown in table 1.
1 eluent gradient of table elutes table
System suitability is investigated:
Mixed reference substance solution and each 5 μ L of test solution is taken to be surveyed with UPLC-PDA under above-mentioned chromatographic condition respectively It is fixed, chromatogram is obtained, 6 kinds of compounds detach completely with other substance peaks, see Fig. 1.
2.4.2 linear relationship is investigated
It is accurate respectively to draw aforementioned 1,2,4,6,8,10 μ L of mixed reference substance solution by above-mentioned chromatographic condition measurement, with sample introduction Amount is abscissa, and peak area is ordinate drawing curve, the results are shown in Table 2.
2 regression equation of table and the range of linearity
Precision Experiment:
Take same test solution, continuous sample introduction 6 times calculates ursin, chlorogenic acid, galuteolin, 3,5-Dicaffeoylquinic acid, different The RSD of chlorogenic acid B and 4,5-Dicaffeoylquinic acid peak area is respectively 0.82%, 1.9%, 1.7%, 1.4%, 1.5%, 1.3%, as a result Illustrate that instrument precision is good.Same sample is taken, is different 3 days and handles respectively, sample introduction is analyzed, 6 ingredient ursin of calculating, The peak area RSD of chlorogenic acid, galuteolin, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid and 4,5-Dicaffeoylquinic acid, result 0.79%, 1.1%, 1.5%, 2.4%, 2.6%, 1.6%.
Repeated experiment:
6 parts of same lot number medicinal material is taken, it is accurately weighed, test solution is prepared by aforementioned test solution preparation method, point It does not measure.Ursin, chlorogenic acid, galuteolin, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid and 4,5-Dicaffeoylquinic acid are flat in 6 parts of test solutions Equal content is respectively 0.728%, 0.0671%, 0.0197%, 0.0278%, 0.142%, 0.0390%, RSD points of content results Not Wei 1.7%, 2.3%, 2.3%, 1.7%, 1.0%, 1.8%, show repeated good.
Stability experiment:
Prepare test solution by aforementioned test solution preparation method respectively, respectively at 0,2,4,8,12, for 24 hours respectively into Sample measures each index components ursin, chlorogenic acid, galuteolin, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid and 4,5-Dicaffeoylquinic acid peak area. Calculate peak area RSD, respectively 1.8%, 1.6%, 1.4%, 1.2%, 1.9%, 1.4%, illustrate that sample solution is small 0 to 24 When it is interior be stable.
Sample recovery rate is tested:
50%9 parts of sampling amount in aforementioned test solution preparation method are weighed, repeatability in pilose gerbera herb is pressed respectively and surveys It is background values to obtain each component content, is separately added into 50%, 100%, 150% reference substance solution, each horizontal respectively by aforementioned Test solution preparation method prepares 3 parts of test solutions, and the rate of recovery of 6 ingredients is measured and calculated by aforementioned chromatographic condition, It the results are shown in Table 3.Ursin average recovery rate 99.69%, RSD (%) are 1.7%, chlorogenic acid average recovery rate 100.9%, RSD (%) is 1.9%, galuteolin average recovery rate 99.92%, and RSD (%) is 1.8%, 3,5-Dicaffeoylquinic acid average recovery rate 100.7%, RSD (%) are 1.2%, 3,4-Dicaffeoylquinic acid average recovery rate 101.1%, RSD (%) is 1.9%, and 4,5-Dicaffeoylquinic acid is flat The equal rate of recovery 99.80%, RSD (%) are 2.0%, show that 6 components recoveries to be measured are good.
3 sample recovery rate experimental result of table
Sample measures
The pilose gerbera herb of Guizhou different sources is collected, and using the method having built up to ursin, chlorogenic acid, reseda Glycosides, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid and 4,5-Dicaffeoylquinic acid ingredient carry out assay, and the results are shown in Table 4.
The content (%, n=2) of 6 kinds of ingredients in 4 different batches pilose gerbera herb of table
From the foregoing, it will be observed that the method for the present invention can make pilose gerbera herb medicinal material Content of Chlorogenic Acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, different Chlorogenic acid C, galuteolin and ursin are preferably detached, and this method is easy, accurate, reproducible, and it is big to can be used for hair The assay of fourth herbal medicine material Content of Chlorogenic Acid, 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, galuteolin and ursin is The quality control of pilose gerbera herb provides reference frame.
Finally it is pointed out that above example is only the more representational example of the present invention.Obviously, technology of the invention Scheme is not limited to above-described embodiment, and acceptable there are many deformations.Those skilled in the art can be from disclosed by the invention All deformations that content is directly exported or associated, are considered as protection scope of the present invention.

Claims (7)

1. a kind of method of Multiple components assay in pilose gerbera herb medicinal material, for measure simultaneously pilose gerbera herb Content of Chlorogenic Acid, The content of 3,5-Dicaffeoylquinic acid, 3,4-Dicaffeoylquinic acid, 4,5-Dicaffeoylquinic acid, galuteolin and ursin, which is characterized in that use UPLC-PDA Method is measured, with WatersBETC18(2.1 × 150mm, 1.7 μm) is chromatographic column, and -0.1% aqueous formic acid of acetonitrile carries out Gradient elution, while utilizing Detection wavelength 280nm and 328nm, flow velocity 0.28mL/min, 40 DEG C of column temperature.
2. the method for Multiple components assay in pilose gerbera herb medicinal material according to claim 1, which is characterized in that described UPLC-PDA methods are used as test solution after diluting pilose gerbera herb herbal extract.
3. the method for Multiple components assay in pilose gerbera herb medicinal material according to claim 2, which is characterized in that described Pilose gerbera herb herbal extract is to extract to obtain to pilose gerbera herb medicinal material using methanol as solvent.
4. the method for Multiple components assay in pilose gerbera herb medicinal material according to claim 3, which is characterized in that described Pilose gerbera herb medicinal material is extracted using methanol as solvent, is that refluxing extraction is carried out to pilose gerbera herb medicinal material with 50% methanol, is returned Stream extraction time is 2h.
5. the method for Multiple components assay in pilose gerbera herb medicinal material according to claim 2, which is characterized in that described Dilution is that pilose gerbera herb herbal extract is diluted 5 times with distilled water.
6. the method for Multiple components assay in pilose gerbera herb medicinal material according to claim 2, which is characterized in that described Pilose gerbera herb medicinal material was the pilose gerbera herb medicinal powder of No. three sieves.
7. the method for Multiple components assay in pilose gerbera herb medicinal material according to claim 1, which is characterized in that described UPLC-PDA methods, wherein test solution are prepared via a method which:Took the pilose gerbera herb medicinal powder of No. three sieves 0.5g, and it is accurately weighed, it sets in conical flask with cover, 50% methanol 25mL is added in precision, and weighed weight is heated to reflux 2 hours, puts It is cold, then weighed weight, the weight of less loss is supplied with 50% methanol, is shaken up, is filtered, and is measured subsequent filtrate 5ml, is transferred to 25ml capacity In bottle, it is diluted to scale with distilled water, is shaken up to get test solution.
CN201810313063.0A 2018-04-09 2018-04-09 method for measuring contents of multiple components in gerbera piloselloides medicinal material Expired - Fee Related CN108490095B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201810313063.0A CN108490095B (en) 2018-04-09 2018-04-09 method for measuring contents of multiple components in gerbera piloselloides medicinal material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201810313063.0A CN108490095B (en) 2018-04-09 2018-04-09 method for measuring contents of multiple components in gerbera piloselloides medicinal material

Publications (2)

Publication Number Publication Date
CN108490095A true CN108490095A (en) 2018-09-04
CN108490095B CN108490095B (en) 2020-01-31

Family

ID=63315193

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201810313063.0A Expired - Fee Related CN108490095B (en) 2018-04-09 2018-04-09 method for measuring contents of multiple components in gerbera piloselloides medicinal material

Country Status (1)

Country Link
CN (1) CN108490095B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113884613A (en) * 2021-08-31 2022-01-04 贵州医科大学 Dactylicapnos tomentosa herb pharmacokinetic analysis method
CN115656399A (en) * 2022-11-07 2023-01-31 江苏卫生健康职业学院 Method for detecting content of active substances in traditional Chinese medicine extraction waste residues

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113884613A (en) * 2021-08-31 2022-01-04 贵州医科大学 Dactylicapnos tomentosa herb pharmacokinetic analysis method
CN115656399A (en) * 2022-11-07 2023-01-31 江苏卫生健康职业学院 Method for detecting content of active substances in traditional Chinese medicine extraction waste residues

Also Published As

Publication number Publication date
CN108490095B (en) 2020-01-31

Similar Documents

Publication Publication Date Title
CN105606734A (en) Method for detecting honeysuckle flower and lonicerae flos medicinal materials through rapid resolution liquid chromatography
CN104777249B (en) The method measuring effective ingredient amygdaloside content in cough syrup of loquat leaf
CN108169386B (en) Method for constructing HPLC (high Performance liquid chromatography) characteristic spectrum of Jingyaokang capsule
CN106706812A (en) Method for detecting bufadienolide components in Liushen pill
CN106124639A (en) The multicomponent content assaying method of Eucommia ulmoides
CN107064322A (en) Gallic acid and the HPLC wavelength of sanguisorbin I contents switching method in garden burnet or garden burnet class preparation are determined simultaneously
CN110927311B (en) Construction method of UPLC (ultra performance liquid chromatography) characteristic spectrum of dogbane leaf medicinal material and method for measuring content of flavonoid component of dogbane leaf medicinal material
CN109521103A (en) A kind of three Le slurry oral solution quality determining method having both qualitative and quantitative evaluation
CN108490095A (en) A kind of method of Multiple components assay in pilose gerbera herb medicinal material
CN111487347A (en) Method for detecting fingerprint of Zhishu granules
CN101788537B (en) Method for measuring content of ellagic acid ingredients in euscaphis japonica medicinal materials
CN107315058A (en) A kind of method of total ginkgoic acid in detection ginkgo biloba succi
CN105510488B (en) A kind of finger-print and its quality determining method for relieving pain patch
CN112798724B (en) Method for establishing chromatographic fingerprint of saponins component suitable for ginseng traditional Chinese medicine and medicinal material extract
CN108663440B (en) Method for constructing UPLC fingerprint spectrum of callicarpa nudiflora medicinal material and standard fingerprint spectrum
CN106290645B (en) A kind of construction method and its standard finger-print of Lhasa rhubarb finger-print
CN104849384B (en) Set up method and its application of strong diisopropyl amine dichloro acetate preparation finger
CN108254470A (en) In glutinous rehmannia while carbohydrate content measure and its fingerprint map construction method
CN107576743A (en) The method for building up and its finger-print of the peaceful spray finger-print of nose
CN104634911B (en) A kind of 4 kinds of flavonoids effective constituent detection methods of CHUANKEZHI ZHUSHEYE
CN107607665A (en) One seedling medicine subprostrate sophora and its Chinese medicine preparation method of quality control
CN113759010B (en) Method for constructing Chinese rose flower characteristic map
CN107976494B (en) Construction of standard characteristic spectrum of Kangfu tincture and quality detection method thereof
CN103837627A (en) Fingerprint spectrum establishment method of groundnut stem and leaf medicinal material
CN111189952A (en) Method for measuring special content of verbena and controlling quality of verbena

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20200131