CN102183604A - Method and application for building fingerprint of cortex fraxini or extract thereof - Google Patents
Method and application for building fingerprint of cortex fraxini or extract thereof Download PDFInfo
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- CN102183604A CN102183604A CN2011100256508A CN201110025650A CN102183604A CN 102183604 A CN102183604 A CN 102183604A CN 2011100256508 A CN2011100256508 A CN 2011100256508A CN 201110025650 A CN201110025650 A CN 201110025650A CN 102183604 A CN102183604 A CN 102183604A
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Abstract
The invention discloses a method for building fingerprint of cortex fraxini or extract thereof by using high-performance capillary electrophoresis (HPCE), comprising the following steps: (a) preparing solution for tests: adding organic solvent into cortex fraxini or extract thereof to extract and dilute to certain volume to obtain the solution for tests; (b) preparing referent solution; preparing daidzein solution as internal standard; (c) conducting electrophoretic analysis conditions: using dihydric phosphate-borax as buffer stock solution and adopting the pH value of the solution between 7.8-9.2, preferably 8.6, using acetonitrile as organic modifier, leading detection wavelength to be within the range of 200-400nm, preferably 210nm, leading working voltage to be within the range of 5-30 kV, preferably 20kV; (d) implementing measuring method: taking sample solution to be analyzed of appropriate amount to sequentially fill into sample bottles and make HPCE measurement, and recording electrophoretic image; and (e) conducting data analysis: calculating the relative migration time of each spectral peak by taking 1 as the retaining time of the internal standard, and calculating the relative peak area of each spectral peak by taking 1 as the peak area of the internal standard. The invention provides a novel method for rapidly, effectively identifying counterfeit and inferior cortex fraxini or extract thereof on markets and differentiating commercial drugs of different production regions.
Description
Technical field
The present invention relates to a kind of method for building up of traditional Chinese medicine fingerprint, specifically, relate to the method for building up and the application of bark of ash medicinal material or its extract HPCE finger-print.
Background technology
The bark of ash makes a variation because of ground, and cultivar origin is different, and (Oleaceae) Ash belongs to (Fraxinus) plant but all belong to Oleaceae, and its morphological feature and smell and book on Chinese herbal medicine are contained similar.Regulation bark of ash of Pharmacopoeia of the People's Republic of China version in 2010 is dry branch skin or the dry hide of congener fraxinus rhynchophylla Hance Fraxinusrhynchophylla Hance, Chinese ash Fraxinus chinensis Roxb., sharp leaf Chinese ash Fraxinus szabaona Lingelsh. or place post Chinese ash Fraxinus stylosa Lingelsh..Wherein fraxinus rhynchophylla Hance is distributed in ground such as Jilin, Liaoning, Hebei, Henan.Chinese ash is distributed in North China, northwest, East China, Central-South, southwest and Liaoning.Point leaf Chinese ash is distributed in Hebei, Shaanxi, Shanxi, Gansu, Hunan.The post Chinese ash is distributed in Shaanxi in the place.The commodity medicinal material mainly comprises the northeast bark of ash or Liaoning bark of ash (fraxinus rhynchophylla Hance), the Sichuan bark of ash (Chinese ash), the Shaanxi white point bark of ash (place post Chinese ash), Henan bark of ash etc.
The effect that the bark of ash has is clearing heat and detoxicating, clear liver and improve vision is used for hot dysentery, has loose bowels, leukorrhea with reddish discharge, red eye, swell pain, order give birth to diseases such as screen film.Modern pharmacological research shows, the bark of ash has that resisting pathogenic microbes, anti-inflammatory, diuresis, anti-freezing and antiallergy, cough-relieving apophlegmatic are relievingd asthma, maincenter suppresses, multiple effect such as antitumor, clinical available bacillary dysentery, chronic bronchitis, the conjunctivitis etc. controlled.
The bark of ash mainly contains coumarin compounds such as aesculin, aesculetin, fraxin, fraxetin, and the Ji Yuan of Chinese Pharmacopoeia regulation bark of ash medicinal material comprises 4 kinds of sweet-scented osmanthus section Ash platymisciums.Because the bark of ash is a how basic source kind, add the geographical environment difference that former plant distributes, cause the commodity quality of medicinal material in the different places of production, source to differ greatly, the bark of ash and mixed pseudo-medicinal material kind are also complicated simultaneously, demand clarification urgently.Therefore, set up a kind of objective, comprehensive, to estimate the method for its inherent quality fast very important.So far, bark of ash Control of Internal Quality adopts the content assaying method of aesculin and aesculetin mostly, only one piece of document has related to the bark of ash finger-print research that more can disclose inherent quality, but should research adopt the HPLC method, there is analysis time long (75min), many deficiencies such as organic solvent consumption is many, and is big for environment pollution.For this reason, the invention provides with HPCE the fingerprint map construction method of the bark of ash medicinal material or its extract that are analysis means, for comprehensive control of bark of ash inherent quality provides new analysis means, to reach the fake and forged commodity product and the purpose of distinguishing different producing regions commodity medicinal material of differentiating the bark of ash on the market or its extract more fast and effectively.
Summary of the invention
One aspect of the present invention relates to the method that a kind of HPCE of use sets up bark of ash medicinal material or its extract finger-print, it is characterized in that may further comprise the steps:
(a) preparation of need testing solution: get bark of ash medicinal material or its extract, add organic solvent extraction, constant volume is need testing solution;
(b) preparation of object of reference solution: preparation Daidzein solution is as interior mark;
(c) electrophoretic analysis condition: with dihydric phosphate-borax is the buffering stock solution, and its pH value is preferably 8.6 between 7.8-9.2; With the acetonitrile is organic modifiers; Detect wavelength between 200-400nm, be preferably 210nm; Operating voltage is preferably 20kV between 5-30kV;
(d) assay method: it is an amount of to get sample solution to be analyzed, and the sample bottle of packing into is successively also gone up HPCE and measured, record electrophoresis spectrogram;
(e) data analysis: the retention time with internal standard compound is 1, calculates the relative migration time respectively compose the peak, is 1 with the peak area of internal standard compound, calculates the relative peak area of respectively composing the peak.
In an embodiment of the invention, the organic solvent in the step (a) is the lower alcohol of C1-C6, is preferably methyl alcohol, more preferably refluxing extraction or ultrasonic Extraction.
In an embodiment of the invention, the concentration of the dihydric phosphate that uses during wherein preparation buffering stock solution is 80-120mmol/L, be preferably 100mmol/L, borax soln concentration is 30-70mmol/L, be preferably 50mmol/L, the volume proportion of two kinds of solution is 2: 1-1: 4, be preferably 1.02: 1.98.
In an embodiment of the invention, buffering stock solution during chromatographic run: water: the volume proportion of organic modifiers is 1.5: 1: 0.2-4: 1: 1, be preferably 3: 1: 0.8.
On the other hand, the invention still further relates to the application of bark of ash finger-print in bark of ash medicinal material or the detection of its extract quality, it is characterized in that with the Daidzein internal standard compound be the reference peak,, be respectively comprising 4 characteristic peaks:
No. 7 peaks, the relative migration time 0.905, RSD 0.52%;
No. 8 peaks, the relative migration time 0.926, RSD 0.41%;
No. 11 peaks, the relative migration time 1.077, RSD 1.21%;
No. 15 peaks, the relative migration time 1.168, RSD 1.51%;
In an embodiment of the invention, described bark of ash finger-print also comprises one or more characteristic peaks, and described characteristic peak is selected from:
No. 1 peak, the relative migration time 0.600, RSD 3.24%;
No. 2 peaks, the relative migration time 0.764, RSD 1.41%;
No. 3 peaks, the relative migration time 0.773, RSD 1.38%;
No. 4 peaks, the relative migration time 0.800, RSD 1.14%;
No. 5 peaks, the relative migration time 0.809, RSD 1.04%;
No. 6 peaks, the relative migration time 0.879, RSD 0.73%;
No. 10 peaks, the relative migration time 1.024, RSD 0.85%;
No. 12 peaks, the relative migration time 1.096, RSD 1.08%;
No. 13 peaks, the relative migration time 1.121, RSD 1.51%;
No. 14 peaks, the relative migration time 1.145, RSD 1.66%;
No. 16 peaks, the relative migration time 1.187, RSD 1.61%.
The invention still further relates to the application of described bark of ash finger-print in bark of ash medicinal material or the detection of its extract quality.
In an embodiment of the invention, described quality testing is meant that the contrast HPCE finger-print similarity of the bark of ash medicinal material to be detected that obtains with the inventive method or its extract HPCE finger-print and control medicinal material or its extract is more than 90%, preferably more than 95%.Described similarity is meant that its electrophoresis spectrogram separately imports the 2004A of Chinese Pharmacopoeia Commission version chromatographic fingerprints of Chinese materia medica similarity evaluation system-computed with the AIA document form and obtains.
Description of drawings
Fig. 1 bark of ash medicinal materials fingerprint, wherein No. 9 peaks are interior mark peak;
The reference fingerprint that 0 batch of bark of ash of Figure 22 is derived, wherein No. 9 peaks are interior mark peak;
Fig. 3 bark of ash 3D chromatogram.
Embodiment
Sample is collected between year March in March, 2005～2007, and except that Qianwei County, Sichuan sample is collect in the place of production, all the other samples purchase all that different in each city pharmacy is different with medicinal material market manages a little.The big pharmacy of same retail is bought once at interval half a year, and per season of medicinal material wholesale market is bought once, buys 5 different businessmans at every turn, and its place of production is provided by businessman.Bark of ash medicinal material details see the following form.
Table 1 sample source
Experimental technique
1 instrument, reagent and sample
U.S. Agilent 3DCE capillary electrophoresis apparatus (model: G1600A comprises diode array detector and HP chromatographic work station); Fused quartz kapillary effective length 45cm (53.5cm * 75 μ m ID, Hebei sharp Feng chromatogram Yongnian device company limited).
Microfuge 18 desk centrifuges (U.S. Beckman Coulter Inc.); Ripple reaches 1004 type ultrasonic cleaners (Shenzhen ripple reaches ultrasonic engineering equipment company limited); TGL.16G table model high speed centrifuge (Shanghai medical analytical instrument factory); BP210D type 100,000/electronic analytical balance (German Sai Duolisi); Milli-Q Superpure water machine (U.S. Millipore company); Filtration unit and miillpore filter (0.45 μ m).
The preparation of 2 solution
2.1 buffer preparation
Accurately take by weighing 1.3609g KH
2PO
4In the 100mL small beaker, in the 100mL measuring bottle, be mixed with the potassium dihydrogen phosphate buffer solution that concentration is 100mmol/L with suitable quantity of water dissolving back constant volume.
Accurately take by weighing 1.9068g sodium tetraborate (Na
2B
4O
710H
2O) in the 100mL small beaker, in the 100mL measuring bottle, be mixed with the borax buffer solution that concentration is 50mmol/L with suitable quantity of water dissolving back constant volume.
Accurate 100mmol/L potassium dihydrogen phosphate and the 50mmol/L borax soln drawn was in 1.02: 1.98 ratio preparation potassium dihydrogen phosphate-borax buffer solution (pH=8.6) storing solutions.Face the time spent and prepare runtime buffer solution: buffering stock solution-water-acetonitrile (3: 1: 0.8) in following ratio.
2.2 reference substance solution preparation
The preparation of inner mark solution: accurately take by weighing Daidzein 100mg in the 100mL small beaker, in the 100mL measuring bottle, be mixed with the solution that every 1mL contains Daidzein 1mg with constant volume behind an amount of dissolve with methanol.
The preparation of reference substance storing solution: precision takes by weighing reference substance fraxin 4.8mg, aesculin 5.6mg, fraxetin 1.96mg, aesculetin 3.76mg respectively, put in the 25mL measuring bottle, add an amount of methyl alcohol ultrasonic dissolution and be diluted to scale, shake up, in contrast product mixing storing solution (1～4 be respectively 192.0,224.0,78.4,150.4mg/L).
Reference substance solution preparation: the accurate reference substance storing solution 5mL that draws, put in the 10mL measuring bottle, add methyl alcohol and be diluted to scale, mixing is drawn 5mL again, put in the 10mL measuring bottle, add inner mark solution 1mL, thin up is to scale, mixing, cross 0.45 μ m miillpore filter, in contrast product solution (1～4 be respectively 48.0,56.0,19.6,37.6mg/L).
2.3 the preparation of control medicinal material and need testing solution
Get bark of ash control medicinal material and test sample powder to be checked No. 3, pharmacopeia (cross sieve) 0.25g, accurately claim surely, put in the tool plug conical flask, the accurate methyl alcohol 25mL that adds, ultrasonic 60min is put coldly, filters.Precision is measured subsequent filtrate 5mL, puts in the 10mL measuring bottle, adds inner mark solution 1mL, and thin up is to scale, mixing, and it is standby to cross 0.45 μ m miillpore filter.
3 detection methods
Before kapillary uses, respectively wash 10～20min (55 ℃) with 0.1mol/L NaOH solution, water, operation buffer solution [100mmol/L potassium dihydrogen phosphate-50mmol/L borax-water-acetonitrile (1.02: 1.98: 1: 0.8)].Wash 1,2 between each sample introduction more respectively, 3min, to guarantee good reappearance.Reference substance, control medicinal material solution and the need testing solution of getting preparation are positioned in the sample bottle, put into injector successively.Detecting wavelength 210nm, pressure sample introduction 20kPas, working voltage 20kV (+)-(-) measures its electrophoresis spectrogram under 25 ℃ of conditions of column temperature.
The checking of 4 methodologies
For investigating the reliability of analytical approach, the bark of ash medicinal material of buying with Chengdu Tongrentang (Chinese ash) is an analytic sample, the precision of instrument analytical method, sample stability, experimental technique repeatability etc. have been carried out corresponding research, and the result shows that this method meets the technical requirement of finger-print (seeing Table 2).
Table 2 precision, stability, repeated similarity Excel computed in software result
5 experimental results
This finger-print is determined 15 total peaks altogether shown in accompanying drawing 1, accompanying drawing 2.Other has the interior mark peak of No. 9 peaks for adding.By relative migration time and standard addition method, determine that wherein No. 7 peaks are the fraxin peak; No. 8 peaks are the aesculin peak; No. 9 internal standard compound matter Daidzeins of peak for adding, this peak is as the reference peak; No. 11 peaks are the fraxetin peak; No. 15 peaks are the aesculetin peak, and the finger-print data are referring to table 3 and table 4.
The three-dimensional collection of illustrative plates of the online collection bark of ash (accompanying drawing 3), by 3D figure and contour map intuitively as seen, near 210nm bark of ash electrophoresis spectrogram peak number is maximum, and the uv absorption wavelength testing result of fraxin, aesculin, fraxetin and 4 kinds of compositions of aesculetin shows in the bark of ash, and the maximum absorption wavelength of each component mainly concentrates near 210nm and the 365nm.Must follow the quantity of information maximization principle in line with the finger-print wavelength determination, further the chromatogram that 190～400nm wavelength is scanned is down analyzed comparison, 210nm place peak number order is more and separate good as a result, not only can demonstrate fully the information of active component, the information that can also reflect other compositions in the medicinal material, can synthetically estimate the quality of the bark of ash more comprehensively, so be to detect wavelength to measure its finger-print with 210nm.
The relative migration time at the total peak of 20 batches of barks of ash of table 3
Remarks: "-" representative does not detect
Continuous table 3
The relative peak area and the similarity at the total peak of 20 batches of barks of ash of table 4
Remarks: "-" representative does not detect; Amount to the bark of ash characteristic peak relative peak area of representative except that interior mark with; r
IrBe related coefficient; C
IrBe included angle cosine.
Continuous table 4
Claims (8)
1. method of using HPCE to set up bark of ash medicinal material or its extract finger-print is characterized in that may further comprise the steps:
(a) preparation of need testing solution: get bark of ash medicinal material or its extract, add organic solvent extraction, constant volume is need testing solution;
(b) preparation of object of reference solution: preparation Daidzein solution is as interior mark;
(c) electrophoretic analysis condition: with dihydric phosphate-borax is the buffering stock solution, and its pH value is preferably 8.6 between 7.8-9.2; With the acetonitrile is organic modifiers; Detect wavelength between 200-400nm, be preferably 210nm; Operating voltage is preferably 20kV between 5-30kV;
(d) assay method: it is an amount of to get sample solution to be analyzed, and the sample bottle of packing into is successively also gone up HPCE and measured, record electrophoresis spectrogram;
(e) data analysis: the retention time with internal standard compound is 1, calculates the relative migration time respectively compose the peak, is 1 with the peak area of internal standard compound, calculates the relative peak area of respectively composing the peak.
2. the method for setting up finger-print according to claim 1, wherein the organic solvent in the step (a) is the lower alcohol of C1-C6, is preferably methyl alcohol, more preferably refluxing extraction or ultrasonic Extraction.
3. the method for setting up finger-print according to claim 1, the concentration of the dihydric phosphate that uses during wherein preparation buffering stock solution is 80-120mmol/L, be preferably 100mmol/L, borax soln concentration is 30-70mmol/L, be preferably 50mmol/L, the volume proportion of two kinds of solution is 2: 1-1: 4, be preferably 1.02: 1.98.
4. the method for setting up finger-print according to claim 3, buffering stock solution during the HPCE operation: water: the volume proportion of organic modifiers is 1.5: 1: 0.2-4: 1: 1, be preferably 3: 1: 0.8.
5. the application of bark of ash finger-print in bark of ash medicinal material or the detection of its extract quality is characterized in that with the Daidzein internal standard compound be the reference peak, comprising 4 characteristic peaks, is respectively:
No. 7 peaks, the relative migration time 0.905, RSD 0.52%;
No. 8 peaks, the relative migration time 0.926, RSD 0.41%;
No. 11 peaks, the relative migration time 1.077, RSD 1.21%;
No. 15 peaks, the relative migration time 1.168, RSD 1.51%;
6. application according to claim 5, described bark of ash finger-print also comprises one or more characteristic peaks, described characteristic peak is selected from:
No. 1 peak, the relative migration time 0.600, RSD 3.24%;
No. 2 peaks, the relative migration time 0.764, RSD 1.41%;
No. 3 peaks, the relative migration time 0.773, RSD 1.38%;
No. 4 peaks, the relative migration time 0.800, RSD 1.14%;
No. 5 peaks, the relative migration time 0.809, RSD 1.04%;
No. 6 peaks, the relative migration time 0.879, RSD 0.73%;
No. 10 peaks, the relative migration time 1.024, RSD 0.85%;
No. 12 peaks, the relative migration time 1.096, RSD 1.08%;
No. 13 peaks, the relative migration time 1.121, RSD 1.51%;
No. 14 peaks, the relative migration time 1.145, RSD 1.66%;
No. 16 peaks, the relative migration time 1.187, RSD 1.61%.
7. the application of any bark of ash finger-print of being set up of claim 1-4 in bark of ash medicinal material or the detection of its extract quality.
8. application according to claim 7, described quality testing is meant with the described detection method of claim 1 step a～d medicinal material to be detected or its extract is analyzed, the any bark of ash finger-print of being set up of HPCE collection of illustrative plates that is obtained and claim 1-4 carries out similarity relatively, described similarity is more than 80%, preferably more than 90%, further preferably more than 95%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109001336A (en) * | 2018-09-20 | 2018-12-14 | 哈尔滨珍宝制药有限公司 | Qinpi Extracts characteristic spectrum, its method for building up and quality determining method |
| CN109917048A (en) * | 2019-04-18 | 2019-06-21 | 江阴天江药业有限公司 | A kind of construction method of the UPLC characteristic spectrum of bark of ash medicinal material, the characteristic spectrum constructed by this method and its application |
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| CN101708233A (en) * | 2009-12-18 | 2010-05-19 | 上海现代中医药技术发展有限公司 | Finger print quality detecting method by intermediates of salvia miltiorrhiza, peach kernels and gynostemma pentaphylla for strengthening body resistance and dissolving stasis |
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| CN101708233A (en) * | 2009-12-18 | 2010-05-19 | 上海现代中医药技术发展有限公司 | Finger print quality detecting method by intermediates of salvia miltiorrhiza, peach kernels and gynostemma pentaphylla for strengthening body resistance and dissolving stasis |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109001336A (en) * | 2018-09-20 | 2018-12-14 | 哈尔滨珍宝制药有限公司 | Qinpi Extracts characteristic spectrum, its method for building up and quality determining method |
| CN109917048A (en) * | 2019-04-18 | 2019-06-21 | 江阴天江药业有限公司 | A kind of construction method of the UPLC characteristic spectrum of bark of ash medicinal material, the characteristic spectrum constructed by this method and its application |
| CN109917048B (en) * | 2019-04-18 | 2022-03-08 | 江阴天江药业有限公司 | Construction method and application of UPLC characteristic spectrum of cortex fraxini medicinal material |
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