CN101518616A - Quality control method for Kouyangqing granules and application thereof - Google Patents
Quality control method for Kouyangqing granules and application thereof Download PDFInfo
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Abstract
The invention discloses a quality control method for Kouyanqing granules, which comprises the following steps: preparing and mixing a reference substance solution; preparing a methanol solution of the Kouyanqing granules as a test solution; analyzing the reference substance solution and the test solution by a high performance liquid chromatography to obtain a high efficiency liquid chromatography finger print of the Kouyanqing granules; and comparing and monitoring the quality of the Kouyanqing granules according to a chromatogram map of the reference substance solution and a finger print of the test solution. The invention also discloses application of the quality control method in identifying the Kouyanqing granules. The quality control method adopts the high efficiency liquid chromatography to establish the finger print of the Kouyanqing granules, and can monitor the stability of technical processes for producing semi-finished products and finished products through the established standard finger print. The method effectively avoids counterfeiting of products, ensures normal production and circulation order of the products, and has outstanding practicability.
Description
Technical field
The present invention relates to a kind of quality control method for Kouyanqing granules and application, specifically is a kind of by making up the quality control method for Kouyanqing granules and the application of finger printing, belongs to the pharmaceutical analysis technical field.
Background technology
Compound preparation with " monarch, minister, help, make " mutual restriction and coordination, emphasize to play a role on the whole, mostly not at certain target spot, simple adduction that neither some compositions, only depend on the detection of single component to reduce the accurate and specificity of differentiating, can not represent the overall efficacy of Chinese medicine preparation, can not reflect its inherent quality, and can not solve problem such as pseudo-product doping.Chinese medicine fingerprint is a kind of comprehensive, quantifiable chemical identification means, can discern the false from the genuine, and estimates the homogeneity and the stability of raw medicinal material, semi-finished product and end product quality, has embodied the globality and the ambiguity of Chinese medicine effect.In recent years, chromatographic fingerprinting is advocated in the quality evaluation of herbal products energetically abroad.By the peak position at collection of illustrative plates principal character peak, area or ratio reflect the kind of chemical constituent and the characteristic of quantity, distinguish the true from the false effectively, estimate good and bad.The chromatographic fingerprinting analysis becomes the feasible pattern of differentiating Chinese medicine verity and evaluation quality concordance and product stability.
Kouyanqing granules has the effect of clearing away heat and nourishing YIN, removing toxic substances and promoting subsidence of swelling; be used for the oral ulcer due to the hyperactivity of fire caused by deficiency of YIN; be national Chinese medicine protection kind; protection kind number: ZYB20720022230; but the quality standard imperfection of present kouyanqing granules; lack method of quality control comprehensively and effectively, easily by imitated.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that remedies prior art, and purpose is to provide a kind of quality control method for Kouyanqing granules effectively reliably.
Another object of the present invention provides the application of above-mentioned control method.
The present invention is achieved through the following technical solutions above-mentioned purpose:
A kind of quality control method for Kouyanqing granules may further comprise the steps:
(1) preparation contains the mixing reference substance solution of chlorogenic acid, caffeic acid, luteoloside, cinnamic acid, liquirtin and ammonium glycyrrhizinate, and each component concentrations is 0.2mg/ml; Preparation kouyanqing granules methanol solution is as need testing solution;
(2) adopt above-mentioned reference substance solution of high-efficient liquid phase chromatogram technique analysis and need testing solution, chromatographic condition is: sample size 10～20 μ l; Chromatographic column is ODS C
18, 250mm * 4.6mm, 5 μ m; Mobile phase is 3.0 water-acetonitrile for transferring to pH with formic acid or acetic acid or phosphoric acid or trifluoroacetic acid, gradient elution; Detect wavelength: 254nm; Obtain the kouyanqing granules efficient liquid-phase chromatograph finger print atlas;
Described gradient elution step is: 0～15 minute, the mobile phase acetonitrile-water faded to 10:90 by 2:98; 15～120 minutes, the mobile phase acetonitrile-water faded to 41:59 by 10:90; 120～125 minutes mobile phase acetonitrile-waters are 41:59;
(3) according to the quality of the finger printing monitoring kouyanqing granules of the chromatogram of reference substance solution and need testing solution.
The described preparation kouyanqing granules of above-mentioned method of quality control step (1) methanol solution is: get kouyanqing granules, with methanol or ethanol extraction, filter, extracting solution reclaims solvent, residue is transferred to solid-phase extraction column after with water dissolution, use water wash, discard leacheate, the described solid-phase extraction column of reuse methanol gradation eluting, collect eluent, reclaim methanol, residue reuse dissolve with methanol is made need testing solution.More specifically, this step is:
Get 10 bags of this product minimum packages, the mixing porphyrize is got about 5～20g, the accurate title, decide, and puts in the tool plug conical flask, accurate methanol or the ethanol 25～100ml of adding, close plug claims to decide weight, supersound process 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol or ethanol, shake up, filter, precision is measured subsequent filtrate 10ml, decompression and solvent recovery is to doing, and residue adds the about 5ml dissolving of water, quantitatively is transferred to solid phase extraction column (filler: ODS C
18, specification: 6ml 500mg), adds water 15ml gradation drip washing, leacheate discards, and reuse methanol 15ml gradation eluting is collected eluent, and decompression and solvent recovery is to doing, residue quantitatively adds methanol 2ml, makes dissolving fully, filters with 0.45 μ m microporous filter membrane, as the finished product need testing solution.
Also free list 1 expression of the step of described gradient elution:
Table 1 gradient elution table
According to method of the present invention, by efficient liquid-phase chromatograph finger print atlas that the 10 batches of kouyanqing granuleses are made up and analyze comparison, find out its common characteristic peak, mark the retention time Rt at each common characteristic peak, obtain the kouyanqing granules standard finger-print.Its total peak is 23, its retention time Rt value is respectively 26min, 28min, 29min, 33min, 37min, 40min, 49min, 51min, 52min, 57min, 59min, 60min, 62min, 64min, 67min, 71min, 72min, 77min, 79min, 98min, 107min, 109min, 114min, and wherein the Rt value is that 7 chromatographic peaks of 28min, 33min, 49min, 52min, 77min, 79min, 114min are chlorogenic acid, caffeic acid, liquirtin, luteoloside, harpagoside, cinnamic acid, ammonium glycyrrhizinate through conclusive evidence.Above chromatographic peak has constituted the fingerprint characteristic of kouyanqing granules.
Quality method provided by the invention can be applied to differentiate kouyanqing granules.
Compared with prior art, the present invention has following beneficial effect:
Kouyanqing granules proper mass standard is recorded in 2005 the version Pharmacopoeia of the People's Republic of China (one one), and [discriminating] is contrast with Radix Glycyrrhizae control medicinal material, Flos Lonicerae control medicinal material respectively, carries out thin layer and differentiate; Chlorogenic acid contents in [assay] employing high effective liquid chromatography for measuring Chinese medicine honeysuckle, not to its inherent chemical constituent carry out comprehensively, systematic research, the detection index is single, easily by imitated, so method of the present invention has been set up the fingerprint pattern technology standard of kouyanqing granules, by have that it's too late feature, the quality of overall monitor semi-finished product and finished product effectively at total peak in the finger printing, monitor the stability of production technology, guarantee stable, the homogeneous, controlled of its quality.The present invention also has method advanced person, stability and advantages such as favorable reproducibility, operability.
The present invention adopts high performance liquid chromatography to make up the finger printing of kouyanqing granules, but utilize the quality of high performance liquid chromatography fingerprint characteristic overall monitor kouyanqing granules, and can monitor the stability of semi-finished product and finished product production process by the standard finger-print of setting up.The present invention has improved kouyanqing granules finished product, half-finished quality monitoring standard, has effectively avoided product counterfeiting, guarantees ordinary production, the circulation order of this kind.
Description of drawings
Fig. 1 is a kouyanqing granules standard finger-print of the present invention, and from left to right arrow indication is respectively a characteristic peak 1 to 23 among the figure.
Fig. 2 mixes the reference substance chromatogram corresponding with the kouyanqing granules finger printing, and peak numbers 1,2,3,4,5,6,7 is designated as chlorogenic acid, caffeic acid, liquirtin, luteoloside, harpagoside, cinnamic acid, ammonium glycyrrhizinate successively among the figure.
Fig. 3 is kouyanqing granules, lacks Flos Lonicerae feminine gender, Flos Lonicerae medical material contrast color spectrogram, and from left to right arrow indication is the peak number that belongs to the chromatographic peak of Flos Lonicerae in the kouyanqing granules finger printing among the figure.
Fig. 4 is kouyanqing granules, lacks Radix Scrophulariae feminine gender, Radix Scrophulariae medical material contrast color spectrogram, and from left to right arrow indication is the peak number that belongs to the chromatographic peak of Radix Scrophulariae in the kouyanqing granules finger printing among the figure.
Fig. 5 kouyanqing granules, lack Radix Glycyrrhizae feminine gender, licorice medicinal materials contrast color spectrogram, from left to right arrow indication is the peak number that belongs to the chromatographic peak of Radix Glycyrrhizae in the kouyanqing granules finger printing among the figure.
The specific embodiment
Below further specify technical scheme of the present invention by specific embodiment.
1 instrument and reagent
1.1 instrument: wear peace Dionex company's high performance liquid chromatograph (ASI-100 automatic sampler, ATH-585 column oven, P680 quaternary gradient pump, PDA-100 detector); Chromatographic column: Dikma PLATISILODS (250mm * 4.6mm, 5 μ m).
1.2 reagent: 10 batches of finished products and corresponding semi-finished product provide by Guangzhou Baiyunshan Heji Huangpu Chinese Medicine Co., Ltd..Liquid chromatograph agents useful for same acetonitrile is chromatographically pure in the experiment, and all the other agents useful for same are analytical pure, and water is ultra-pure water.
2. method and result
2.1 the preparation of need testing solution: get 10 bags of this product respectively, porphyrize is got about 10g, and accurate the title decides, put in the tool plug conical flask accurate methanol (or ethanol) 50ml, the close plug of adding, claim to decide weight, supersound process (power 360W, frequency 35kHz) 30 minutes, put coldly, claim again to decide weight, or ethanol is supplied the weight that subtracts mistake, shake up, filter, precision is measured subsequent filtrate 10ml, decompression and solvent recovery is to doing, and residue adds the about 5ml dissolving of water, quantitatively is transferred to solid phase extraction column (filler: C
18, specification: 6ml 500mg), adds water 15ml gradation drip washing, leacheate discards, and reuse methanol 15ml gradation eluting is collected eluent, and decompression and solvent recovery is to doing, residue quantitatively adds methanol 2ml, makes dissolving fully, filters with 0.45 μ m microporous filter membrane, as the finished product need testing solution.
The preparation of semi-finished product need testing solution: get the about 0.6g of this product runny plaste, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 50ml that adds, close plug claims to decide weight, supersound process (power 360W, frequency 35kHz) 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, filtrate decompression reclaims solvent to doing, residue adds the about 5ml dissolving of water, quantitatively is transferred to solid phase extraction column (filler: C18, specification: 6ml, 500mg), add water 15ml gradation drip washing, leacheate discards, reuse methanol 15ml gradation eluting, collect eluent, decompression and solvent recovery is to doing, and residue quantitatively adds methanol 2ml, makes dissolving fully, filter with 0.45 μ m microporous filter membrane, as the semi-finished product need testing solution.
Mix the preparation of reference substance solution: take by weighing chlorogenic acid, caffeic acid, luteoloside, cinnamic acid, liquirtin, the about 2mg of ammonium glycyrrhizinate reference substance respectively, the accurate title, decide, in the 10ml measuring bottle, make the mixing reference substance solution that every ml contains chlorogenic acid, caffeic acid, luteoloside, cinnamic acid, liquirtin, each 0.2mg of ammonium glycyrrhizinate with methanol constant volume.
Following medicinal material coarse powder is respectively got in the preparation of three flavor medical material need testing solutions, Flos Lonicerae 1g, Radix Scrophulariae 0.8g, licorice medicinal materials 0.5g, the accurate title, decide, place round-bottomed flask respectively, add 50% ethanol 50ml, reflux, extract, 2 hours, filter, filtrate decompression is concentrated into dried, and residue adds the about 5ml dissolving of water, quantitatively is transferred to SPE solid phase extraction column (filler: C
18, specification: 6ml 500mg), adds water 15ml gradation drip washing, leacheate discards, and reuse methanol 15ml gradation eluting is collected eluent, and decompression and solvent recovery is to doing, residue dissolves with small amount of methanol, is settled to 10ml, with the microporous filter membrane filtration of 0.45 μ m, as the medical material need testing solution.
2.2 efficient liquid phase chromatographic analysis: accurate finished product and semi-finished product need testing solution 15 μ l, the sample introduction drawn; Chromatographic condition: chromatographic column is Dikma PLATISIL ODS C18,250mm * 4.6mm, 5 μ m; Mobile phase is acetonitrile (A)-0.1% formic acid solution (B), adopts the gradient elution mode of table 2:
Table 2 gradient elution table
Detect wavelength: 254nm; Flow velocity: 0.8ml/min; Obtain the kouyanqing granules efficient liquid-phase chromatograph finger print atlas.
2.3 total peak is determined: the efficient liquid-phase chromatograph finger print atlas of above-mentioned 10 batches of kouyanqing granuleses that obtain is compared through " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system version ", and common pattern (with reference to finger printing) occurs 23 altogether.Its retention time Rt value is respectively 26min, 28min, 29min, 33min, 37min, 40min, 49min, 51min, 52min, 57min, 59min, 60min, 62min, 64min, 67min, 71min, 72min, 77min, 79min, 98min, 107min, 109min, 114min; In 23 common characteristic peaks, the chromatographic peak that belongs to Flos Lonicerae has 12, and the chromatographic peak that belongs to Radix Scrophulariae has 4, and the chromatographic peak that belongs to Radix Glycyrrhizae should have 8; Wherein the Rt value is that 7 chromatographic peaks of 28min, 33min, 49min, 52min, 77min, 79min, 114min are chlorogenic acid, caffeic acid, liquirtin, luteoloside, harpagoside, cinnamic acid, ammonium glycyrrhizinate through conclusive evidence; The chromatographic peak of 77min is that Radix Glycyrrhizae and Radix Scrophulariae are total, and they have constituted the fingerprint characteristic of kouyanqing granules, can be used as the standard finger-print of kouyanqing granules, specifically see accompanying drawing 1, wherein the chromatographic peak of 77min is two undivided chromatographic peaks, and we are classified as a peak with it, is decided to be the peak No. 18.
Contrast mixes reference substance chromatogram (A) and kouyanqing granules standard finger-print (B), has determined 7 compositions in the kouyanqing granules, specifically sees Fig. 2, and A is for mixing reference substance among the figure, and B is a kouyanqing granules.
Contrast Flos Lonicerae medical material contrast color spectrogram (A) and kouyanqing granules standard finger-print (C), there are 12 chromatographic peaks corresponding in the kouyanqing granules standard finger-print with Flos Lonicerae medical material contrast chromatograph, all there are not this 12 chromatographic peaks and lack in the negative chromatogram of Flos Lonicerae (B), specifically see Fig. 3, A is the Flos Lonicerae medical material among the figure, B is for lacking the Flos Lonicerae feminine gender, and C is a kouyanqing granules, determines that thus these 12 chromatographic peaks belong to Flos Lonicerae fully in the kouyanqing granules standard finger-print.
Contrast Radix Scrophulariae medical material contrast color spectrogram (A) and kouyanqing granules standard finger-print (B), there are 4 chromatographic peaks corresponding in the kouyanqing granules standard finger-print with Radix Scrophulariae medical material contrast chromatograph, and lack in the negative chromatogram of Radix Scrophulariae (C), except No. 18 chromatographic peaks, there are not all the other 3 chromatographic peaks, concrete accompanying drawing 4, A is the Radix Scrophulariae medical material among the figure, B is a kouyanqing granules, and C determines thus that for lacking the negative control of Radix Scrophulariae these 3 chromatographic peaks belong to Radix Scrophulariae fully.
Contrast licorice medicinal materials contrast color spectrogram (A) and kouyanqing granules standard finger-print (C), there are 8 chromatographic peaks corresponding in the kouyanqing granules standard finger-print with Radix Scrophulariae medical material contrast chromatograph, and lack in the negative chromatogram of Radix Glycyrrhizae (B), except No. 18 chromatographic peaks, there are not all the other 7 chromatographic peaks, specifically see Fig. 5, A is a licorice medicinal materials among the figure, B is for lacking the negative control of Radix Glycyrrhizae, and C is a kouyanqing granules, determines that thus these 7 chromatographic peaks belong to Radix Glycyrrhizae fully.No. 18 peaks (being the 77min chromatographic peak) are that Radix Scrophulariae and Radix Glycyrrhizae are common, and the composition that wherein belongs to Radix Scrophulariae is defined as harpagoside.
2.4 precision test: get same kouyanqing granules need testing solution continuous sample introduction 6 times, detect finger printing, adopt " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system version " to estimate, the result shows the need testing solution similarity all greater than 0.999, and the precision of instrument is good.Precision the results are shown in Table 3:
Table 3 precision result
| S1 | S2 | S3 | S4 | S5 | S6 | Reference fingerprint | |
| S1 | 1.000 | 1.000 | 0.999 | 1.000 | 0.999 | 1.000 | 1.000 |
| S2 | 1.000 | 1.000 | 0.999 | 1.000 | 0.999 | 1.000 | 1.000 |
| S3 | 0.999 | 0.999 | 1.000 | 0.999 | 1.000 | 0.999 | 1.000 |
| S4 | 1.000 | 1.000 | 0.999 | 1.000 | 0.999 | 1.000 | 1.000 |
| S5 | 0.999 | 0.999 | 1.000 | 0.999 | 1.000 | 0.999 | 1.000 |
| S6 | 1.000 | 1.000 | 0.999 | 1.000 | 0.999 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 |
2.5 study on the stability: get same kouyanqing granules need testing solution, respectively at 0,3,6,9,12,24,48 hour sample introduction, detect finger printing, adopt " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system version " to estimate, the result shows the need testing solution similarity all greater than 0.999, need testing solution place in 48 hours stable.Stability result sees Table 4:
Table 4 stability result
| Interval (h) | S1(0) | S2(3) | S3(6) | S4(9) | S5(12) | S6(24) | S7(48) | Reference fingerprint |
| S1(0) | 1.000 | 1.000 | 0.999 | 0.999 | 0.999 | 0.999 | 1.000 | 1.000 |
| S2(3) | 1.000 | 1.000 | 0.999 | 0.999 | 0.999 | 0.999 | 1.000 | 1.000 |
| S3(6) | 0.999 | 0.999 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 0.999 |
| S4(9) | 0.999 | 0.999 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 0.999 |
| S5(12) | 0.999 | 0.999 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 0.999 |
| S6(24) | 0.999 | 0.999 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 0.999 |
| S7(48) | 1.000 | 1.000 | 0.999 | 0.999 | 0.999 | 0.999 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 1.000 |
2.6 replica test: get with 6 parts of a collection of kouyanqing granules test samples, by " preparation of a finished product and semi-finished product need testing solution " below method preparation, the difference sample introduction, detect finger printing, adopt " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system version " to estimate, the result shows the need testing solution similarity all greater than 0.950, the method good reproducibility.The results are shown in Table 5:
Table 5 stability result
| S1 | S2 | S3 | S4 | S5 | S6 | Reference fingerprint | |
| S1 | 1.000 | 0.980 | 0.986 | 0.960 | 0.975 | 0.986 | 0.978 |
| S2 | 0.980 | 1.000 | 0.999 | 0.994 | 0.999 | 0.999 | 1.000 |
| S3 | 0.986 | 0.999 | 1.000 | 0.990 | 0.996 | 1.000 | 0.998 |
| S4 | 0.960 | 0.994 | 0.990 | 1.000 | 0.996 | 0.990 | 0.995 |
| S5 | 0.975 | 0.999 | 0.996 | 0.996 | 1.000 | 0.996 | 1.000 |
| S6 | 0.986 | 0.999 | 1.000 | 0.990 | 0.996 | 1.000 | 0.998 |
| Reference fingerprint | 0.978 | 1.000 | 0.998 | 0.995 | 1.000 | 0.998 | 1.000 |
2.7 middle precision: precision takes by weighing the kouyanqing granules of same lot number, respectively under variable such as same date, different analysts condition not, measure in accordance with the law, detect finger printing, adopt " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system version " to estimate.
2.7.1 different analysis times: get same lot number kouyanqing granules, respectively at same date not by " preparation of finished product and semi-finished product need testing solution " below method preparation manipulation, sample introduction, detect finger printing, adopt " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system version " to estimate, the result shows that the need testing solution similarity is all greater than 0.999.Similarity result sees Table 6:
Table 6 similarity result
| S1 (date 1) | S2 (date 2) | Reference fingerprint | |
| S1 (date 1) | 1.000 | 0.998 | 1.000 |
| S2 (date 2) | 0.998 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 |
2.7.2 different analysts: get same lot number kouyanqing granules, different personnel are respectively by " preparation of a finished product and semi-finished product need testing solution " below method preparation manipulation, sample introduction, detect finger printing, adopt " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system version " to estimate, the result shows that the need testing solution similarity is all greater than 0.999.Similarity result sees Table 7:
Table 7 similarity result
| S1 (personnel 1) | S2 (personnel 2) | Reference fingerprint | |
| S1 (personnel 1) | 1.000 | 0.999 | 1.000 |
| S2 (personnel 2) | 0.999 | 1.000 | 1.000 |
| Reference fingerprint | 1.000 | 1.000 | 1.000 |
Claims (4)
1. quality control method for Kouyanqing granules may further comprise the steps:
(1) preparation contains the mixing reference substance solution of chlorogenic acid, caffeic acid, luteoloside, cinnamic acid, liquirtin and ammonium glycyrrhizinate, and each component concentrations is 0.2mg/ml; Preparation kouyanqing granules methanol solution is as need testing solution;
(2) adopt above-mentioned reference substance solution of high-efficient liquid phase chromatogram technique analysis and need testing solution, chromatographic condition is: sample size 10～20 μ l; Chromatographic column is ODS C
18, 5 μ m; Mobile phase is water-acetonitrile of 3.0 for transfer to pH with formic acid or acetic acid or phosphoric acid or trifluoroacetic acid, gradient elution; Detect wavelength: 254nm; Obtain the kouyanqing granules efficient liquid-phase chromatograph finger print atlas;
Described gradient elution step is: 0～15 minute, the mobile phase acetonitrile: water faded to 10:90 by 2:98; 15～120 minutes, the mobile phase acetonitrile: water faded to 41:59 by 10:90; 120～125 minutes mobile phase acetonitriles: water is 41:59;
(3) relatively and according to the quality of the finger printing monitoring kouyanqing granules of the chromatogram of reference substance solution and need testing solution.
2. method of quality control as claimed in claim 1 is characterized in that the kouyanqing granules of preparation described in the step (1) methanol solution is: get kouyanqing granules, with methanol or ethanol extraction, filter, methanol extract liquid reclaims solvent, and residue is transferred to solid-phase extraction column after with water dissolution, uses water wash, discard leacheate, the described solid-phase extraction column of reuse methanol gradation eluting is collected eluent, reclaims methanol, residue reuse dissolve with methanol is made need testing solution.
3. method of quality control as claimed in claim 1, it is characterized in that finger printing has 23 characteristic peaks described in step (2) and the step (3), the retention time of each characteristic peak is respectively 26min, 28min, 29min, 33min, 37min, 40min, 49min, 51min, 52min, 57min, 59min, 60min, 62min, 64min, 67min, 71min, 72min, 77min, 79min, 98min, 107min, 109min, 114min, wherein retention time is 28min, 33min, 49min, 52min, 77min, 79min, 7 chromatographic peaks of 114min successively with the chromatogram of reference substance solution in chlorogenic acid, caffeic acid, liquirtin, luteoloside, harpagoside, cinnamic acid, ammonium glycyrrhizinate is identical.
4. the application of the described method of quality control of claim 1 is to be applied to differentiate kouyanqing granules.
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