CN103245733A - Identification method for wrinkled giant hyssop drip pills - Google Patents
Identification method for wrinkled giant hyssop drip pills Download PDFInfo
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- CN103245733A CN103245733A CN2012100243201A CN201210024320A CN103245733A CN 103245733 A CN103245733 A CN 103245733A CN 2012100243201 A CN2012100243201 A CN 2012100243201A CN 201210024320 A CN201210024320 A CN 201210024320A CN 103245733 A CN103245733 A CN 103245733A
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Abstract
The invention relates to an identification method for wrinkled giant hyssop drip pills. The identification method comprises the following steps of step 1, preparation of a finger-print spectrum of standard wrinkled giant hyssop drip pills; step 2, preparation of a finger-print spectrum of to-be-identified wrinkled giant hyssop drip pills; and step 3, comparison of similarity of the finger-print spectra, and if the finger-print spectra are similar, the wrinkled giant hyssop drip pills are qualified.
Description
Technical field
The present invention relates to field of medicaments, be specifically related to a kind of authentication method of ageratum dripping pill.
Background technology
The ageratum dripping pill is the exclusive kind that Tianjin Tasly Pharmaceutical Co., Ltd produces, modern Chinese herbal medicine as sky scholar's power research and development represents formulation, characteristics such as having the medicine stability height, be difficult for hydrolysis oxidation, rapid-action, free from extraneous odour, mouthfeel are good, easy to carry.Said preparation is the compound preparation that comprises 10 flavor medicinal materials compositions of patchouli oil, rhizoma atractylodis, dried orange peel, the bark of official magnolia, and only wherein patchouli oil, the root of Dahurain angelica, the bark of official magnolia 3 flavor medicinal materials are qualitatively or quantitatively determined in the existing detection method, can not reflect the quality condition of product comprehensively.According to consulting pertinent literature and intra-company's data, find in the dried orange peel in aurantiamarin, the bark of official magnolia in magnolol-honokiol, the root of Dahurain angelica that composition detection wavelength such as Imperatorin-Isomperatorin is all close.Through experimental study, find the mode by the conversion wavelength, 11 main chromatographic peaks all can reach separation requirement in the product, thus the invention provides a kind of authentication method of ageratum dripping pill finger-print, for the quality control of said preparation provides more perfect detection method.
For realizing this purpose, the present invention is by the research to ageratum dripping pill efficient liquid-phase chromatograph finger print atlas, a kind of better ageratum dripping pill method of quality control has been proposed, remedied the deficiency of existing Quality Control Technology, further improved the quality control level of this product, the quality control of product is improved and science more.
Summary of the invention:
Technical matters to be solved
The object of the invention is to provide a kind of ageratum dripping pill finger print atlas identifying method, and the resulting ageratum dripping pill of method standard finger-print thus.
Technical scheme
The invention provides a kind of ageratum dripping pill finger print atlas identifying method, this method may further comprise the steps:
The preparation of step 1, standard ageratum dripping pill finger-print;
The preparation of step 2, ageratum dripping pill finger-print to be measured;
Step 3, the similarity of finger-print is compared, both are similar to show that ageratum dripping pill to be measured is qualified.
Wherein, described ageratum dripping pill is made by rhizoma atractylodis 80-240g, dried orange peel 80-240g, bark of official magnolia 80-240g, root of Dahurain angelica 120-360g, Poria cocos 120-360g, shell of areca nut 120-360g, living tuber of pinellia 80-240g, extract of licorice root 10-30g, patchouli oil 0.8-2.4ml, perilla leaf oil 0.4-1.2ml and appropriate amount of auxiliary materials.
Preferred ageratum pill prescription is as follows:
1) get rhizoma atractylodis 160g, dried orange peel 160g, bark of official magnolia 160g, root of Dahurain angelica 240g, Poria cocos 240g, shell of areca nut 240g, to give birth to tuber of pinellia 160g, extract of licorice root 20g, patchouli oil 1.6mL and perilla leaf oil 0.8mL standby;
2) above ten flavors, get rhizoma atractylodis, dried orange peel, the bark of official magnolia, the root of Dahurain angelica respectively according to the percolation under liquid extract and the extract item (2000 editions appendix 1O of Chinese Pharmacopoeia), make solvent with 60% ethanol, flood and carry out diacolation after 24 hours, collect the about 8000mL of percolate, recovery ethanol, soup are standby; After Poria cocos added water boil, 80 ℃ of temperature were soaked secondary, and 3 hours for the first time, 2 hours for the second time, merge warm immersion liquid, filter filtrate for later use; Give birth to tuber of pinellia cold water soak, changed water one time in per 8 hours, bubble is to the saturating heart, and other adds rhizoma zingiberis 13.5g, the boiling secondary, and 3 hours for the first time, 2 hours for the second time, collecting decoction filtered filtrate for later use; Shell of areca nut boiling 3 hours filters, and filtrate and above-mentioned filter liquid and filtrate merging are concentrated into the thick paste shape, add extract of licorice root, patchouli oil and perilla leaf oil, mixing.Get an amount of polyglycol-6000, heating makes fusion, adds above-mentioned thick paste, stirs evenly, and makes dripping pill 1025g, the bag film-coating, namely.
Wherein, described step 1, the preparation of standard ageratum dripping pill finger-print, method is as follows:
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing (power 200W, frequency 40kHz) 10-30 minute, preferred 15 minutes, put cold, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely.
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram, wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and preferred ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and optimum condition sees Table 1; Flow velocity is 0.1-0.4ml/min, preferred 0.2ml/min; Column temperature is 20-0 ℃, preferred 30 ℃; Sample size is 1-3 μ L, preferred 1 μ L; The detection wavelength is 254mn-336nm, and the optimal wavelength switching condition sees Table 2;
Table 1 gradient elution table
Table 2 wavelength switching condition table
According to chromatogram, discovery has 11 peaks, wherein, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, the relative retention time of other 10 chromatographic peaks is respectively: 0.930,1.293,1.332,1.693,2.311,2.378,2.417,2.510,2.571,2.967, the relative retention time at each peak is utilized computer simulation similarity software for calculation 2004A version in ± 3%, match determines to obtain ageratum dripping pill standard control finger-print.
Wherein, the preparation method of step 2 ageratum dripping pill to be measured finger-print, step is as follows;
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing (power 200W, frequency 40kHz) 10-30 minute, preferred 15 minutes, put cold, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.Solution is injected high performance liquid chromatograph, obtain chromatogram.
Chromatographic condition wherein is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and preferred ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and optimum condition sees Table 1; Flow velocity is 0.1-0.4ml/min, preferred 0.2ml/min; Column temperature is 20-40 ℃, preferred 30 ℃; Sample size is 1-3 μ L, preferred 1 μ L; The detection wavelength is 254mn-336nm, and the optimal wavelength switching condition sees Table 2;
Table 1 gradient elution table
Table 2 wavelength switching condition table
The ageratum dripping pill finger-print that step 1 and step 2 are obtained relatively, similarity be 0.90 or more for qualified, similarity be more than 0.95 for conforming to, similarity is to be identical more than 0.98.
The present invention also provides from above-mentioned finger-print relative method and derives and another next ageratum dripping pill authentication method, and this method may further comprise the steps:
The preparation of step 1, standard ageratum dripping pill finger-print;
The preparation of step 2, ageratum dripping pill finger-print to be measured;
Step 3, the retention time of 6 main peaks on the finger-print is compared; Wherein, described step 1, the preparation of standard ageratum dripping pill finger-print, method is as follows:
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely;
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram, wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
After analyzing relatively to the finger-print of 10 batches of ageratum dripping pills, 6 main chromatographic peaks have been determined, in the chromatogram, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, compare with No. 2 peak retention times, the retention time at all the other 5 peaks is respectively: 0.931,1.689,2.369,2.560,2.954; Be characteristic peak with above-mentioned 6 peaks in the finger-print, obtain standard ageratum dripping pill finger-print;
Wherein, the preparation method of step 2 ageratum dripping pill to be measured finger-print, step is as follows;
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.Solution is injected high performance liquid chromatograph, obtains chromatogram,
Wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
Wherein, the retention time of 6 main peaks compares on step 3, the finger-print that step 1 and step 2 are obtained; Step is as follows; The chromatographic peak identical with reference substance peak retention time is No. 2 peaks, compare with No. 2 peak retention times, the relative retention time of other 5 chromatographic peaks is respectively 0.931 (No. 1 peak), 1.689 (No. 3 peaks), 2.369 (No. 4 peaks), 2.560 (No. 5 peaks), 2.954 (No. 6 peaks).On the finger-print to be measured on the relative retention time at 6 peaks and the standard finger-print relative retention time at 6 peaks be that product to be tested is qualified ± 3% with in.
The present invention is by the foundation of above finger-print, further established the authentication method of ageratum dripping pill, adopt this method can accurately distinguish the ageratum dripping pill, according to the comparison of standard finger-print, draw the discriminating conclusion, more and standard finger-print approaching, product quality is more good, and similarity can use computer approach to confirm, is for qualified more than 0.90 as similarity, similarity be more than 0.95 for conforming to, similarity is for identical more than 0.98.
The said method particularly preparation method of the standard control finger-print of ageratum dripping pill obtains through screening, below is screening process:
1.1 instrument and reagent
Instrument: U.S. Waters H-CLASS, Empower2 workstation.
Chromatographic column: ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um);
Reagent: methyl alcohol (chromatographically pure, Tianjin Concord Technology Co., Ltd.); Acetonitrile (chromatographically pure, German MERK company); Glacial acetic acid (analyze pure, Tianjin Chemical Reagents Factory No.1); Water is ultrapure water.
Reference substance: aurantiamarin (lot number: 110721-201014, assay usefulness is by 95.1% purity meter);
Magnolol
(lot number: 110729-200411, assay is used); Honokiol (lot number: 110730-201011, assay usefulness is by 98.4% purity meter); Liquiritin (lot number: 111610-200503, assay is used); Ammonium glycyrrhetate (lot number: 110731-200615, assay is used); Imperatorin (lot number: 0826-200206, assay is used); Isomperatorin (lot number: 110827-200407, differentiate with) is Nat'l Pharmaceutical ﹠ Biological Products Control Institute to be provided; Atisine chloride Atractydin (Tianjin one side scientific ﹠ technical corporation provides)
Sample: (Tianjin Tasly Pharmaceutical Co., Ltd, totally 19 batches, concrete lot number sees Table 3 to the ageratum dripping pill, all is up to the standards through the quality inspection center.
Table 3 sample message table
1.2 the selection of chromatographic condition
1.2.1 detect the selection of wavelength
" Chinese pharmacopoeia and pertinent literature have gathered in the ageratum dripping pill in the 10 flavor medicinal materials and have adopted liquid phase to measure the principal ingredient of content, and search respectively or carry out the ultraviolet full wavelength scanner, determine the maximum absorption wavelength of principal ingredient, see Table 4 with reference to 2010 editions.
Each principal ingredient absorbing wavelength situation of table 4
Information to sum up, preliminary project adopt the mode that wavelength switches to set up analytical approach according to each principal ingredient peak sequence and time.And about principal ingredient absorbing wavelength more than 60% concentrates on absorption is arranged between the 280-295nm, so adopt 294nm to investigate the gradient elution chromatography (GEC) condition, treat tentatively to determine each principal ingredient peak sequence, after the time, further investigate the chromatographic peak situation under 254nm, the 336nm wavelength condition, with the final setting of determining the wavelength switching condition.
1.2.2 the selection of eluent gradient, wavelength switching condition
Measure aurantiamarin in the ageratum dripping pill, magnolol, honokiol content method data simultaneously in conjunction with HPLC method in intra-company's " ageratum dripping pill quality standard draft ", adopt acetonitrile-0.5% glacial acetic acid water system to carry out the investigation of condition of gradient elution, be to detect wavelength with 294nm, determine each principal ingredient peak sequence and time, further determine the wavelength switching condition again.
1.2.2.1 the selection of eluent gradient
With reference to existing data and document, by the adjustment optimization of the phase ratio that flows, determine that condition of gradient elution sees Table 1; Flow velocity: 0.2ml/min; Detect wavelength: 294nm; Column temperature is 30 ℃; Sample size: 3 μ L.
The typical color spectrogram is seen Fig. 1 under this chromatographic condition, and as seen from the figure: have 12 main chromatographic peaks approximately, whole chromatogram is divided into three parts, goes out the peak and mainly concentrate on two time periods, and first concentrates between 8～13min, and 5 chromatographic peaks are arranged approximately; Between second portion 13～20min, chromatographic peak is all very little; Third part concentrates between 20～27min, and 7 chromatographic peaks are arranged approximately.
1.2.2.2 the selection of wavelength switching condition
Use the condition of gradient elution that 1.2.2.1 determines, investigate chromatographic peak situation under 254nm, the 336nm respectively, see Fig. 2,3.
Equally chromatogram under 254nm, the 336nm is divided into three parts, three chromatograms of contrast go out peak number and chromatographic peak size, mark off five groups of chromatographic peaks altogether, analyze and find: first group of chromatographic peak, between 8～10min, with maximum under the 294nm wavelength; Second and third, four groups of chromatographic peaks, between 10～24min, with maximum under the 254nm wavelength; The 5th group of chromatographic peak be obvious chromatographic peak area maximum under 336nm then.
By above analysis result, set the wavelength switching condition, see Table 2.
Then condition of gradient elution and wavelength switching condition are integrated unification, tentatively determine the chromatographic condition of the fingerprint analysis method of ageratum dripping pill, resulting chromatogram is seen Fig. 4.
1.3 the preparation of need testing solution
This product of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing (power 200W, frequency 40kHz) 15 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.Through preliminary reference substance comparison, determine that No. 2 peaks are that aurantiamarin, No. 7 peaks are that honokiol, No. 10 peaks are magnolol.
1.4 the selection of sample size
Find in the process of the test, the symmetry of No. 2 peak aurantiamarins is relatively poor, symmetrical factor only is about 0.80, acromion appears in chromatographic peak behind the magnification ratio, think that then possible cause wraps up in assorted other peak that has for the aurantiamarin chromatographic peak, so condition of gradient elution is carried out suboptimization again, the result does not still have improvement through optimizing repeatedly.When then investigating the old and new's lot number aurantiamarin reference substance solution, find that aurantiamarin reference substance chromatographic peak there are differences because concentration is different, so the sample size of need testing solution is reduced to 1 μ L from 3 μ L, this moment, aurantiamarin chromatographic peak symmetrical factor was 1.06, and chromatographic peak does not have the acromion appearance behind the magnification ratio, determine finally that then sample size is 1 μ L, adopt 1.2 chromatographic condition gained chromatograms after following the integration to see Fig. 5.
1.5 the selection of chromatographic column
Chromatographic column because of the difference of producer, model specification and filler, the filler mode is different can cause bigger influence to the separation case of chromatographic column, so select other 2 kinds of chromatographic columns commonly used for use, investigates comparison.
①ACQUITY?UPLC-BEH?Shield?RP?18(2.1*100mm，1.7um)；
②Agilent?ZORBAX?SB-C18(2.1*100mm，1.8um)；
The result shows that chromatographic column 1. middle small peak separation is relatively poor, sees Fig. 6; Chromatographic column 2. middle chromatographic peak has the phenomenon of losing, and sees Fig. 7.
1.6 determining of liquid phase analysis condition
To sum up analyze, determine that finally ageratum dripping pill fingerprint map analyzing liquid-phase condition is as follows:
Chromatographic column: ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Phase flows: condition of gradient elution sees Table 3; Flow velocity: 0.2ml/min; Column temperature is 30 ℃; Sample size: 1 μ L; Detect wavelength: the wavelength switching condition sees Table 4.
1.7 the selection with reference to the peak reaches definite
Chromatographic peak in the sample finger-print is positioned with reference substance by 1.6 following chromatographic conditions, correspondence goes out 6 kinds of compositions altogether, see Fig. 8, analyze and find that 6 kinds of compositions all belong to flavones ingredient, and it is the highest with content of hesperidin, so determine with aurantiamarin to be with reference to the peak, the aurantiamarin reference substance is provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number is 110721-201014, assay usefulness is by 95.1% purity meter.
The preparation of object of reference solution: it is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely.
1.8 the methodology checking of finger-print test
1.8.1 replica test
Get that (lot number: 110803), by " 1.3 " operation down, 6 parts of test samples of parallel preparation adopt " 1.6 " down chromatographic condition, analyze with a collection of ageratum dripping pill.
Retention time and peak area with No. 2 peak aurantiamarins are 1, calculate the ratio of relative retention time (R.Rt) and the relative peak area (R.A) of other each total fingerprint peaks.The results are shown in Table 5.Result's repeatability is good.
The repeated relative retention time of table 5, relative peak area tables of data
1.8.2 precision test
Get with a collection of ageratum dripping pill (lot number: 110803), press " 1.3 " operation down, prepare 1 part of test sample continuous sample introduction 6 times, adopt " 1.6 " item chromatographic condition down, analyze.
Retention time and peak area with No. 2 peak aurantiamarins are 1, calculate the ratio of relative retention time (R.Rt) and the relative peak area (R.A) of other each total fingerprint peaks.The results are shown in Table 6.Precision is good as a result.
Table 6 precision relative retention time, relative peak area tables of data
1.8.3 stability test
Get with a collection of ageratum dripping pill (lot number: 110803), by " 1.3 " operation down, prepare 1 part of test sample in 0,2,4,6,8,12,16,20,24H sample introduction respectively, adopt chromatographic condition under " 1.6 ", analyze.
Retention time and peak area with No. 2 peak aurantiamarins are 1, calculate the ratio of relative retention time (R.Rt) and the relative peak area (R.A) of other each total fingerprint peaks.The results are shown in Table 7.Sample stability is good in the 24H as a result.
The stable relative retention time of table 7, relative peak area tables of data
2.1 fingerprint spectrum method analysis
By above definite ageratum dripping pill test sample disposal route and chromatographic condition, 10 batches of ageratum dripping pills of picked at random are pressed " 1.3 " operation down, adopt " 1.6 " item chromatographic condition down, analyze.
2.1.1 the foundation of reference fingerprint
According to 10 batches of given correlation parameters of ageratum dripping pill test sample UPLC collection of illustrative plates, the main chromatographic peak that the ageratum dripping pill is measured gained all occurred in 32 minutes, then by the technical requirement of setting up finger-print, record the need testing solution chromatogram of namely 64 minutes 2 times of times, show 32 minutes and do not occur chromatographic peak later on, see Fig. 9.
Relatively the chromatogram of 10 batch samples finds that it is that each batch is total that 11 chromatographic peaks are arranged, the overlapping chromatogram (see figure 10) of 10 batch samples.In addition relative retention time and the relative peak area at 11 total peaks in 10 batch samples are analyzed, be with reference to the peak with No. 2 peak aurantiamarins, calculate relative retention time and the peak area ratio at other 10 total peaks, then the relative retention time RSD of 10 batch samples is all in 0.1%; Unimodal area all in 5.0%, sees Table 8,9 greater than 10% relative peak area ratio R SD.
Table 810 batch sample relative retention time tables of data
Table 9 10 batch sample relative peak area ratio data tables
2.1.2 determining of reference fingerprint
Be total peak with 11 peaks in the finger-print of above-mentioned 10 batch samples, utilize computer simulation similarity software for calculation (2004A version), ageratum dripping pill reference fingerprint is determined in match, sees Figure 11.
Be contrast with ageratum dripping pill reference fingerprint, adopt computer simulation similarity software for calculation (2004B version), the similarity of precision, repeatability, stability test data in the computing methodology checking, similarity all more than 0.995, the results are shown in Table 10.
The similarity of table 10 precision, repeatability, stability test data
2.1.3 the source attribution analysis at total peak
By test sample preparation method under " 1.3 " item, investigate the finger-print situation of ageratum medicinal extract, ageratum medicinal extract is not for comprising the middle extract of patchouli oil, perilla leaf oil, extract of licorice root, adopt " 1.6 " item chromatographic condition down, analyze, compare with the finger-print of ageratum dripping pill sample, collection of illustrative plates basically identical as a result, chromatographic peak number and highly equal indifference, think at first then in the ageratum dripping pill finger-print that 11 total peaks do not derive from this 3 flavor medicinal material of patchouli oil, perilla leaf oil and Radix Glycyrrhizae, see that wrinkled giant hyssop just
The finger-print comparison diagram of gas medicinal extract and ageratum dripping pill sample, Figure 12.
By test sample preparation method under " 1.3 " item, preparation lacks the negative sample of dried orange peel, the bark of official magnolia, rhizoma atractylodis, the root of Dahurain angelica, the tuber of pinellia, the shell of areca nut, Poria cocos respectively again, by chromatographic condition under " 1.6 " item, analyzes.In conjunction with existing reference substance chromatographic peak qualitatively, determine the source ownership at 11 total peaks under the existence conditions respectively, almost all concentrate on rhizoma atractylodis, dried orange peel, the root of Dahurain angelica, the bark of official magnolia 4 flavor medicinal materials, see Table 11.
The source ownership indicator gauge at table 1111 a total peak
2.1.4 the determining fingerprint pattern of sample
By test sample preparation method under " 1.3 " item, adopt " 1.6 " item chromatographic condition down, the finger-print situation of investigation ageratum dripping pill 9 batch samples is analyzed.Adopt computer simulation similarity software for calculation (2004B version) to calculate similarity, similarity all more than 0.995, sees Table 12 as a result.
The keep sample similarity tables of data of sample of table 12 ageratum dripping pill
2.1.5 the standard of finger-print limits
By above investigation result, tentatively formulate the finger-print similarity of ageratum dripping pill more than 0.95, the follow-up follow-up of quality that also needs a large amount of samples, data accumulation.
2.2 characteristic spectrum methods analyst
By above definite ageratum dripping pill test sample disposal route and chromatographic condition, 10 batches of ageratum dripping pills of picked at random are pressed " 1.3 " operation down, adopt " 1.6 " item chromatographic condition down, analyze.
Selection 6 main peaks wherein carry out the characteristic spectrum analysis of ageratum dripping pill as the characteristic peak of ageratum dripping pill, are foundation with the relative retention time, carry out the data statistic analysis of methodology checking project and 10 batches of on-line sample.Consistent with aurantiamarin reference substance peak retention time is No. 2 peaks, and 6 characteristic peak characteristic spectrums are seen Figure 13.
2.2.1 the replica test of characteristic spectrum
Be with reference to the peak with No. 2 peaks, the relative retention time RSD of other 5 characteristic peaks is all below 0.1%.
The replica test tables of data of table 13 characteristic spectrum
2.2.2 the precision of characteristic spectrum test
Be with reference to the peak with No. 2 peaks, the relative retention time RSD of other 5 characteristic peaks is all below 0.1%.
The precision test figure table of table 14 characteristic spectrum
2.2.3 the stability test of characteristic spectrum
Be with reference to the peak with No. 2 peaks, the relative retention time RSD of other 5 characteristic peaks is all below 0.2%.
The stability test tables of data of table 15 characteristic spectrum
2.2.4 characteristic peak source ownership is investigated
By test sample preparation method under " 1.3 " item, investigate the finger-print situation of ageratum medicinal extract, ageratum medicinal extract is not for comprising patchouli oil, perilla leaf oil, the middle extract of extract of licorice root, adopt " 1.6 " item chromatographic condition down, analyze, compare with the finger-print of ageratum dripping pill sample, collection of illustrative plates basically identical as a result, chromatographic peak number and highly equal indifference, think at first that then 6 characteristic peaks do not derive from patchouli oil in the ageratum dripping pill finger-print, this 3 flavor medicinal material of perilla leaf oil and Radix Glycyrrhizae, see the finger-print comparison diagram of ageratum medicinal extract and ageratum dripping pill sample, Figure 14.
By test sample preparation method under " 1.3 " item, preparation lacks the negative sample of dried orange peel, the bark of official magnolia, rhizoma atractylodis, the root of Dahurain angelica, the tuber of pinellia, the shell of areca nut, Poria cocos respectively again, by chromatographic condition under " 1.6 " item, analyzes.In conjunction with existing reference substance chromatographic peak qualitatively, determine the source ownership of 6 characteristic peaks under the existence conditions respectively, almost all concentrate on rhizoma atractylodis, dried orange peel, the root of Dahurain angelica, the bark of official magnolia 4 flavor medicinal materials, see Table 16.
The source ownership indicator gauge of table 166 characteristic peak
2.2.5 the sample of characteristic spectrum is investigated
The relative retention time analysis of characteristic spectrum is carried out in investigation to 10 batches of above on-line sample and 9 batches of samples that keep sample, as a result in 19 batch samples except No. 2 peaks with reference to 5 characteristic peak RSD the peak all in 0.5%, see Table 17.Then
Table 1719 batch sample relative retention time tables of data
2.2.6 the standard of characteristic spectrum limits
According to the data of above 19 batch sample characteristic spectrums, the standard of tentatively formulating characteristic spectrum limits as described below:
Should present 6 main chromatographic peaks in the test sample chromatogram, the chromatographic peak identical with reference substance peak retention time is No. 2 peaks, compare with No. 2 peak retention times, the relative retention time of other 5 chromatographic peaks is respectively 0.931 (No. 1 peak), 1.689 (No. 3 peaks), 2.369 (No. 4 peaks), 2.560 (No. 5 peaks), 2.954 (No. 6 peaks).The relative retention time at each peak should be in relative retention time ± 3% of regulation.
Beneficial effect of the present invention is:
The present invention is by attempting multiple different elution requirements and wavelength switching condition, determined that finally wavelength switches method is carried out fingerprint map analyzing to the ageratum dripping pill chromatographic condition, the reference fingerprint at 11 total peaks and the standard finger-print of 6 main peaks have been determined in investigation, method is easy, quick, good reproducibility, satisfies related request through the methodology checking.
The fingerprint analysis method of a kind of ageratum dripping pill that should set up with the present invention, carried out fingerprint map analyzing to comprising 9 batch samples in 10 years, result and reference fingerprint are compared and are calculated similarity all more than 0.995, show that this method that the present invention sets up is applicable to the requirements for quality control of product.
The fingerprint analysis method applicability of a kind of ageratum dripping pill that the present invention sets up is strong, can reflect the quality condition of product more comprehensively.
Description of drawings:
Fig. 1 chromatogram, its chromatographic column be ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um), wavelength 294nm
Fig. 2 chromatogram, its chromatographic column be ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um), wavelength 254nm
Fig. 3 chromatogram, its chromatographic column be ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um), wavelength 336nm
Fig. 4 chromatogram, its chromatographic column are that (2.1*100mm, 1.7um), wavelength switches ACQUITY UPLC-HSS T3
Fig. 5 chromatogram, its chromatographic column be ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um), sample size 1 μ L
Fig. 6 chromatogram, its chromatographic column be ACQUITY UPLC--BEH Shield RP 18 (2.1*100mm, 1.7um), sample size 1 μ L
Fig. 7 chromatogram, its chromatographic column be Agilent ZORBAX SB-C18 (2.1*100mm, 1.8um), sample size 1 μ L
Fig. 8 chromatogram, its chromatographic column be ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um), sample size 1 μ L
Figure 92 doubly analyzes the duration chromatogram, its chromatographic column be ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um)
Figure 101 0 batch sample comparison colours spectrogram, its chromatographic column be ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um)
Figure 11 ageratum dripping pill reference fingerprint fitted figure
Figure 12 ageratum medicinal extract and dripping pill sample comparison diagram
The contrast characteristic spectrum of Figure 136 characteristic peak
Figure 14 ageratum medicinal extract and dripping pill sample comparison diagram
Embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1, the determining fingerprint pattern of ageratum dripping pill
Get lot number and be 110803 ageratum dripping pill
Step 1, the preparation of need testing solution
The ageratum dripping pill of getting under the content uniformity item to be measured is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing (power 200W, frequency 40kHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.
Adopt high performance liquid chromatography, chromatographic condition is: and chromatographic column ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and condition sees Table 1; Flow velocity 0.2ml/min; Column temperature is 30 ℃; Sample size 1 μ L; The detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2; Analyze need testing solution with this understanding, obtain the finger-print of ageratum dripping pill to be measured.Embodiment 2, the determining fingerprint pattern of ageratum dripping pill
Get lot number and be 110803 ageratum dripping pill
Step 1, the preparation of need testing solution
The ageratum dripping pill of getting under the content uniformity item to be measured is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing (power 200W, frequency 40kHz) 30 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.
Adopt high performance liquid chromatography, chromatographic condition is: and chromatographic column ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-1% glacial acetic acid buffer solution for gradient elution mutually, and condition sees Table 1; Flow velocity 0.1ml/min; Column temperature is 30 ℃; Sample size 1 μ L; The detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2; Analyze need testing solution with this understanding, obtain the finger-print of ageratum dripping pill to be measured.Embodiment 3, the determining fingerprint pattern of ageratum dripping pill
Get lot number and be 110306 ageratum dripping pill
Step 1, the preparation of need testing solution
The ageratum dripping pill of getting under the content uniformity item to be measured is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing (power 200W, frequency 40kHz) 15 minutes, put coldly, claim to decide weight again, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.
Adopt high performance liquid chromatography, chromatographic condition is: and chromatographic column ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and condition sees Table 1; Flow velocity 0.2ml/min; Column temperature is 30 ℃; Sample size 2 μ L; The detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2; Analyze need testing solution with this understanding, obtain the finger-print of ageratum dripping pill to be measured.
According to method provided by the invention, the UPLC reference fingerprint of setting up with the ageratum dripping pill is contrast, adopts computer simulation similarity software for calculation (2004B version) to calculate, and similarity is 0.997.
Chromatographic condition changes to:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and elution requirement sees Table 1; Flow velocity is 0.4ml/min, and column temperature is 20 ℃, and sample size is 1 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2;
Table 1 gradient elution table
Table 2 wavelength switching condition table
Embodiment 5, the determining fingerprint pattern of ageratum dripping pill
Chromatographic condition changes to:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and elution requirement sees Table 1; Flow velocity is 0.3ml/min, and column temperature is 40 ℃, and sample size is 3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2;
Table 1 gradient elution table
Table 2 wavelength switching condition table
Embodiment 6, the preparation 1 of the finger-print of standard control ageratum dripping pill
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely;
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram, wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
Finger-print to 10 batches of ageratum dripping pills is analyzed comparison, 11 total peaks have been determined, in the chromatogram, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, the relative retention time of other 10 chromatographic peaks is respectively: 0.930,1.293,1.332,1.693,2.311,2.378,2.417,2.510,2.571,2.967, the relative retention time at each peak is in ± 3%, utilize computer simulation similarity software for calculation 2004A version, match determines to obtain ageratum dripping pill standard control finger-print.
Embodiment 7, the preparation 2 of the finger-print of standard control ageratum dripping pill
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing (power 200W, frequency 40kHz) 10～30 minutes, preferred 15 minutes, put cold, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely.
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram, wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing with the octadecylsilane chemically bonded silica be filler ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and elution requirement sees Table 1; Flow velocity is 0.2ml/min; Column temperature is 30 ℃; Sample size is 1 μ L; The detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2;
Table 1 gradient elution table
Table 2 wavelength switching condition table
After analyzing relatively to the finger-print of 10 batches of ageratum dripping pills, 6 main chromatographic peaks have been determined, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, compare with No. 2 peak retention times, the retention time at all the other 5 peaks is respectively: 0.931,1.689,2.369,2.560,2.954, the relative retention time at each peak is in ± 3%, and these total peaks have constituted the fingerprint characteristic of ageratum dripping pill, can be used as the standard control finger-print of ageratum dripping pill.
Step 1, the preparation of standard ageratum dripping pill finger-print, method is as follows:
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely;
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram, wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
Finger-print to 10 batches of ageratum dripping pills is analyzed comparison, 11 total peaks have been determined, in the chromatogram, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, the relative retention time of other 10 chromatographic peaks is respectively: 0.930,1.293,1.332,1.693,2.311,2.378,2.417,2.510,2.571,2.967, the relative retention time at each peak is in ± 3%, utilize computer simulation similarity software for calculation 2004A version, match determines to obtain ageratum dripping pill standard control finger-print.
The preparation method of step 2 ageratum dripping pill to be measured finger-print, step is as follows;
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10～30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely.Solution is injected high performance liquid chromatograph, obtains chromatogram,
Wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
Step 3, the ageratum dripping pill finger-print that step 1 and step 2 are obtained relatively, similarity is to be qualified 0.90 or more.
Claims (10)
1. ageratum dripping pill authentication method is characterized in that this method may further comprise the steps:
The preparation of step 1, standard ageratum dripping pill finger-print;
The preparation of step 2, ageratum dripping pill finger-print to be measured;
Step 3, the similarity of finger-print is compared.
2. according to the authentication method of claim 1, it is characterized in that, wherein, described ageratum dripping pill is made by rhizoma atractylodis 80-240g, dried orange peel 80-240g, bark of official magnolia 80-240g, root of Dahurain angelica 120-360g, Poria cocos 120-360g, shell of areca nut 120-360g, living tuber of pinellia 80-240g, extract of licorice root 10-30g, patchouli oil 0.8-2.4ml, perilla leaf oil 0.4-1.2ml and appropriate amount of auxiliary materials.
3. according to the authentication method of claim 1, it is characterized in that wherein, described ageratum dripping pill is to be prepared from by following method:
1) get rhizoma atractylodis 160g, dried orange peel 160g, bark of official magnolia 160g, root of Dahurain angelica 240g, Poria cocos 240g, shell of areca nut 240g, to give birth to tuber of pinellia 160g, extract of licorice root 20g, patchouli oil 1.6mL and perilla leaf oil 0.8mL standby;
2) above ten flavors are got rhizoma atractylodis, dried orange peel, the bark of official magnolia, the root of Dahurain angelica respectively according to the percolation under liquid extract and the extract item, make solvent with 60% ethanol, and flood and carry out diacolation after 24 hours, the about 8000mL of collection percolate, recovery ethanol, soup are standby; After Poria cocos added water boil, 80 ℃ of temperature were soaked secondary, and 3 hours for the first time, 2 hours for the second time, merge warm immersion liquid, filter filtrate for later use; Give birth to tuber of pinellia cold water soak, changed water one time in per 8 hours, bubble is to the saturating heart, and other adds rhizoma zingiberis 13.5g, the boiling secondary, and 3 hours for the first time, 2 hours for the second time, collecting decoction filtered filtrate for later use; Shell of areca nut boiling 3 hours filters, and filtrate and above-mentioned filter liquid and filtrate merging are concentrated into the thick paste shape, add extract of licorice root, patchouli oil and perilla leaf oil, mixing; Get an amount of polyglycol-6000, heating makes fusion, adds above-mentioned thick paste, stirs evenly, and makes dripping pill 1025g, the bag film-coating, namely.
4. according to the authentication method of claim 1, it is characterized in that,
Wherein, described step 1, the preparation of standard ageratum dripping pill finger-print, method is as follows:
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely;
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram, wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
Finger-print to 10 batches of ageratum dripping pills is analyzed comparison, 11 total peaks have been determined, in the chromatogram, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, the relative retention time of other 10 chromatographic peaks is respectively: 0.930,1.293,1.332,1.693,2.311,2.378,2.417,2.510,2.571,2.967, the relative retention time at each peak is in ± 3%, utilize computer simulation similarity software for calculation 2004A version, match determines to obtain ageratum dripping pill standard control finger-print.
5. according to the authentication method of claim 1, it is characterized in that,
Wherein, the preparation method of step 2 ageratum dripping pill to be measured finger-print, step is as follows;
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely; Solution is injected high performance liquid chromatograph, obtains chromatogram,
Wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
6. according to the authentication method of claim 1, it is characterized in that,
Described step 3, the similarity of finger-print is compared, be ageratum dripping pill finger-print that step 1 and step 2 are obtained relatively, similarity is to be qualified 0.90 or more.
7. according to the authentication method of claim 1, it is characterized in that,
Described step 3, the similarity of finger-print is compared, be ageratum dripping pill finger-print that step 1 and step 2 are obtained relatively, similarity is to be qualified 0.95 or more.
8. according to the authentication method of claim 1, it is characterized in that,
Described step 3, the similarity of finger-print is compared, be ageratum dripping pill finger-print that step 1 and step 2 are obtained relatively, similarity is to be qualified 0.98 or more.
9. according to the authentication method of claim 1, it is characterized in that step is as follows:
Step 1, the preparation of the finger-print of standard control ageratum dripping pill
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely;
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram, wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing with the octadecylsilane chemically bonded silica be filler ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and elution requirement sees Table 1; Flow velocity is 0.2ml/min; Column temperature is 30 ℃; Sample size is 1 μ L; The detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2;
Table 1 gradient elution table
Table 2 wavelength switching condition table
Finger-print to 10 batches of ageratum dripping pills is analyzed comparison, 11 total peaks have been determined, in the chromatogram, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, the relative retention time of other 10 chromatographic peaks is respectively: 0.930,1.293,1.332,1.693,2.311,2.378,2.417,2.510,2.571,2.967, the relative retention time at each peak is in ± 3%, utilize computer simulation similarity software for calculation 2004A version, match determines to obtain ageratum dripping pill standard control finger-print;
Step 2, the determining fingerprint pattern of ageratum dripping pill to be measured
The preparation of need testing solution
The ageratum dripping pill of getting under the content uniformity item to be measured is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
Adopt high performance liquid chromatography, chromatographic condition is: and chromatographic column ACQUITY UPLC-HSS T3 (2.1*100mm, 1.7um); Flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and condition sees Table 1; Flow velocity 0.2ml/min; Column temperature is 30 ℃; Sample size 1 μ L; The detection wavelength is 254mn-336nm, and the wavelength switching condition sees Table 2; Obtain the finger-print of ageratum dripping pill to be measured with this understanding;
Step 3, the ageratum dripping pill finger-print that step 1 and step 2 are obtained relatively, similarity is to be qualified 0.90 or more.
10. ageratum dripping pill authentication method is characterized in that this method may further comprise the steps:
The preparation of step 1, standard ageratum dripping pill finger-print;
The preparation of step 2, ageratum dripping pill finger-print to be measured;
Step 3, the retention time of 6 main peaks on the finger-print is compared;
Wherein, described step 1, the preparation of standard ageratum dripping pill finger-print, method is as follows:
1) preparation of need testing solution,
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely;
2) preparation of reference substance solution, method is as follows:
It is an amount of that precision takes by weighing the aurantiamarin reference substance, adds the methyl alcohol dissolving and make the solution that every 1ml contains 140 μ g, namely;
3) determining of finger-print,
Need testing solution and reference substance solution are injected high performance liquid chromatograph, obtain chromatogram,
Wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
After analyzing relatively to the finger-print of 10 batches of ageratum dripping pills, 6 main chromatographic peaks have been determined, in the chromatogram, the chromatographic peak identical with aurantiamarin reference substance peak retention time is No. 2 peaks, compare with No. 2 peak retention times, the retention time at all the other 5 peaks is respectively: 0.931,1.689,2.369,2.560,2.954;
Wherein, the preparation method of step 2 ageratum dripping pill to be measured finger-print, step is as follows;
The ageratum dripping pill of getting under the content uniformity item is an amount of, crushes dressing, gets about 1g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methyl alcohol 25ml that adds, close plug claims to decide weight, ultrasonic processing 10-30 minute, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methyl alcohol, shake up, filter, get subsequent filtrate, namely; Solution is injected high performance liquid chromatograph, obtains chromatogram,
Wherein the chromatographic condition of high performance liquid chromatography is as follows:
Chromatographic column is fixing to be filler with the octadecylsilane chemically bonded silica, and flowing is acetonitrile-0.5% glacial acetic acid buffer solution for gradient elution mutually, and flow velocity is 0.1-0.4ml/min, column temperature is 20-40 ℃, sample size is 1-3 μ L, and the detection wavelength is 254mn-336nm, and the wavelength switching condition is as follows:
Wherein, step 3, the retention time of 6 main peaks on two finger-prints is compared; Step is as follows; The chromatographic peak identical with reference substance peak retention time is No. 2 peaks, compare with No. 2 peak retention times, the relative retention time of other 5 chromatographic peaks is respectively 0.931,1.689,2.369,2.560,2.954, and the relative retention time at 6 peaks is that product to be tested is qualified ± 3% with on the relative retention time at 6 peaks on the finger-print more to be measured and standard finger-print.
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| CN112213416A (en) * | 2020-09-03 | 2021-01-12 | 广东一方制药有限公司 | Finger print construction method and identification method of two traditional Chinese medicine formula granules |
| CN114636779A (en) * | 2022-03-29 | 2022-06-17 | 陕西科技大学 | Method for constructing sanhua decoction reference sample freeze-dried powder fingerprint spectrum and fingerprint spectrum thereof |
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| CN116183739A (en) * | 2022-11-25 | 2023-05-30 | 河北省药品医疗器械检验研究院(河北省化妆品检验研究中心) | Determination method for analyzing fingerprint of Huoxiang Zhengqi soft capsule |
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