CN101011480B - Method for overall monitoring for kidney-tonifying body-strengthening tablet quality - Google Patents
Method for overall monitoring for kidney-tonifying body-strengthening tablet quality Download PDFInfo
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Abstract
The present invention relates to a method for detecting the quality of kidney tonifying tablet using fingerprints, which comprises the following steps: first, building the standard fingerprint diagram of barren wort, doddor, woodwardic, middle extractum and final tablet; second, checking the fingerprints of tested barren wort, doddor, woodwardic, middle extract and final tablet; third, comparing the fingerprints of the three ingredients to be tested with each standard fingerprint. The groups with met similarity can be used as material to be used in production, and the qualified middle extract is used in next process, and the final tablet is used as final product. The method for detecting the quality of kidney tonifying tablet using fingerprints of the present invention can realize full-process quality monitoring including crude medicine and midbody extractum so that the whole productive technology is more easy to be controlled and the adjustment is more scientific and reasonable, thus eventually obtaining stable and consistant product quality.
Description
Technical field
The present invention relates to a kind of method that detects kidney-tonifying body-strengthening tablet quality with fingerprint pattern technology, comprise the HPLC standard finger-print that makes up epimedium herb, Semen Cuscutae medical material, Rhizoma Cibotii medical material, intermediate extractum and finished tablet respectively, and monitor three flavor medical materials, intermediate extractum, finished tablet method for quality with standard finger-print.
Background technology
BUSHEN QIANGSHEN PIAN is existing national standard medicine.It is made by Herba Epimedii, Fructus Rosae Laevigatae, Fructus Ligustri Lucidi, Semen Cuscutae, Rhizoma Cibotii 5 flavor medicines.Wherein Herba Epimedii, Fructus Rosae Laevigatae, Fructus Ligustri Lucidi decoct with water and are condensed into intermediate extractum; Semen Cuscutae, Rhizoma Cibotii are ground into fine powder, with above-mentioned intermediate extractum and appropriate amount of auxiliary materials mix homogeneously, make tablet again.The quality control key component is that the sugar in the medicine, flavone, saponin component are carried out qualitative identification in the standard of medicine up till now, also comprises the main component in the Herba Epimedii---the qualitative thin layer of icariin is differentiated and the HPLC detection by quantitative.Sugar, flavone, saponin component complexity in medicine are not that single medical material is exclusive, so the general identification experiment that they are carried out, specificity is poor.Chinese medicine preparation mostly is compound recipe, has multitask, many target spots, characteristics such as the onset composition is many, so in the standard only to a composition---icariin carries out qualitative and quantitative detection, not only can not the effective identification medicine true and false, and also very unilateral to the evaluation of drug quality, be difficult to guarantee also whether quality stable between different batches, perhaps with the similar drug in other pharmaceutical factories between whether consistent.
According to the general requirement of production management, it also is far from being enough only monitoring end product quality, should all set up corresponding monitoring means to the important step in the whole process of production.The key component of the national standard quality monitoring of epimedium herb is to the qualitative and quantitative detection of icariin and the total flavones assay in icariin in the punishment of current BUSHEN QIANGSHEN PIAN; The Semen Cuscutae medical material just has only microscopical identification; The Rhizoma Cibotii medical material is that the thin layer of section microscopical identification and protocatechualdehyde, protocatechuic acid is differentiated.These all seem unilateral for estimating quality of medicinal material, are difficult to guarantee the stable, consistent of quality of medicinal material.In addition, the intermediate extractum that produces in the production process does not have national standard, and this is quality monitoring in process of production just.For our pharmaceutical production producer, press for a kind of method that can both quality monitoring in the medicine whole process of production.
Chinese medicine fingerprint is meant spectrum or stratographic collection of illustrative plates common, that have the common composition of distinctive composition in certain Chinese crude drug (extract, Chinese patent medicine).It has used the notion of prudence fingerprint identification, and the utilization modern analytical technique obtains the series of features signal of Chinese crude drug (extract, Chinese patent medicine), and the collection of illustrative plates of being made up of these characteristic signals has individual uniqueness, has represented the feature of measured object.The Chinese medicine fingerprint technology is differentiated the similarities and differences of Chinese crude drug (extract, Chinese patent medicine) from " face " of two dimension, and what emphasize is similarity whole between collection of illustrative plates.Fingerprint pattern technology can be used in the true and false of differentiating Chinese medicine, quality of production monitoring, medical material to the variation of some composition of finished product, the many aspects such as mass discrepancy between the product of the same race, it provides more conventional quality standard deeper quality evaluation pattern, strengthened the controllability of Chinese medicine quality, be the plant amedica quality evaluation pattern of a lot of authorized by states of going abroad.Do not have under the clear and definite situation in the present stage Effective Components of Chinese Herb overwhelming majority, the Chinese medicine fingerprint technology has great importance for the quality of effective control Chinese crude drug (extract, Chinese patent medicine).
At present, Semen Cuscutae and Rhizoma Cibotii medical material are not seen the disposable research report that detects a plurality of compositions and set up finger printing with HPLC.Though epimedium herb has the people to study its finger printing, its detection method is not suitable for this medicine.Intermediate extractum and BUSHEN QIANGSHEN PIAN finished product are not seen the disposable research report that detects a plurality of compositions and set up finger printing with HPLC yet.In order to reach the purpose of omnidistance quality monitoring, the applicant is applied to study in this respect to fingerprint pattern technology.
Summary of the invention
The purpose of this invention is to provide a kind of method that detects kidney-tonifying body-strengthening tablet quality with fingerprint pattern technology, can realize from medical material, to intermediate extractum, arrive the complete monitoring of finished product again, make the easier control of production technology, adjust also more science, rationally, finally make the quality of finished product reach stable, consistent.
Technical solution of the present invention is:
The first step, structure HPLC standard finger-print, method is as follows:
(a), test liquid preparation:
1. take by weighing powder 2.0g in the epimedium herb, in tool plug conical flask, add the 20ml80% methanol solution, supersound extraction 60min is put coldly, filters, and gets subsequent filtrate and filters with 0.45 μ m microporous filter membrane, promptly gets the Herba Epimedii test liquid;
2. take by weighing powder 1.0g in the Semen Cuscutae medical material, other promptly get the Semen Cuscutae test liquid with 1.;
3. take by weighing powder 1.0g in the Rhizoma Cibotii medical material, other promptly get the Rhizoma Cibotii test liquid with 1.;
4. take by weighing intermediate extractum 0.6g, other promptly get intermediate extractum test liquid with 1.;
5. take by weighing BUSHEN QIANGSHEN PIAN finished product fine powder 3.0g, other are same 1., and the tablet test liquid gets product.
(b), chromatographic condition: Agilent 1100 type high performance liquid chromatographs, the DAD detector detects wavelength 350nm; Enlightening horse 200 * 4.6mm, 5 μ m C18 posts; 30 ℃ of column temperatures; Flow velocity 1ml/min; Mobile phase is acetonitrile, 1% acetic acid solution, gradient elution, and the eluting ratio is:
T-min CH3CN％ 1％CH3COOH％
0 5 95
20 5 95
80 45 55
90 5 95
(c), algoscopy: draw above-mentioned test liquid 20ul respectively and inject hplc determination, the chromatogram of record 90min.
10 batches of epimedium herbs are produced in Gansu, 10 batches of Semen Cuscutae medical materials are produced in the Inner Mongol, 10 batches of Rhizoma Cibotii medical materials are produced in Guangxi, 10 batches of intermediate extractum, 10 batches of finished tablets are measured respectively, find out its main common characteristic peak respectively, through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " match, set up HPLC standard colour chart finger printing separately.Be specially:
Epimedium herb has selected 11 main common characteristic peaks altogether, is followed successively by the Y1-Y11 peak, and retention time is respectively: 31.8min, 47.4min, 53.8min, 59.0min, 59.7min, 60.4min, 61.7min, 63.3min, 66.8min, 78.6min, 83.0min.The relative standard deviation RSD% of described 11 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of epimedium herbs and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950.
The Semen Cuscutae medical material is selected 6 main common characteristic peaks altogether, is followed successively by the T1-T6 peak, and retention time is respectively: 31.8min, 44.3min, 46.2min, 46.7min, 50.1min, 68.4min.The relative standard deviation RSD% of described 6 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of Semen Cuscutae medical materials and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.900.
The Rhizoma Cibotii medical material is selected 8 main common characteristic peaks altogether, is followed successively by the G1-G8 peak, and retention time is respectively: 7.4min, 17.2min, 21.3min, 25.4min, 29.8min, 32.9min, 39.3min, 40.9min.The relative standard deviation RSD% of described 8 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of Rhizoma Cibotii medical materials and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950.
Intermediate extractum method for making is that above-mentioned 10 batches of epimedium herbs become 10 batches of intermediate extractum with Fructus Rosae Laevigatae, Fructus Ligustri Lucidi medical material mixing decocting and concentrating respectively, and the weight ratio of every batch three flavor medical material is 161: 97: 97.Intermediate extractum is selected 11 main common characteristic peaks altogether, is Y1 successively, retention time 31.8min; Y2, retention time 47.4min; Y3, retention time 53.8min; Y4, retention time 59.0min; Y5, retention time 59.7min; Y6, retention time 60.4min; Y7, retention time 61.7min; X2, retention time 69.4min; Y10, retention time 78.6min; Y11, retention time 83.0min.The relative standard deviation RSD% of described 11 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of intermediate extractum and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950.
Finished tablet is selected 23 main common characteristic peaks altogether, is successively: G1, retention time 7.4min; G2, retention time 17.2min; G3, retention time 21.3min; G4, retention time 25.4min; G5, retention time 29.8min; X1, retention time 31.8min; G6, retention time 32.9min; G7, retention time 39.3min; G8, retention time 40.9min; T2, retention time 44.3min; T3, retention time 46.2min; T4, retention time 46.7min; Y2, retention time 47.4min; T5, retention time 50.1min; Y3, retention time 53.8min; Y4, retention time 59.0min; Y5, retention time 59.7min; Y6, retention time 60.4min; Y7, retention time 61.7min; T6, retention time 68.4min; X2, retention time 69.5min; Y10, retention time 78.6min; Y11, retention time 83.0min.The relative standard deviation RSD% of described 23 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of finished tablets and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.900.
The characteristic peak of ownership Herba Epimedii is Y1, Y2, Y3, Y4, Y5, Y6, Y7, Y10, Y11 peak in the intermediate extractum standard finger-print, totally 9 peaks; The X2 peak is newly-increased composition.
The characteristic peak of ownership intermediate extractum is Y2, Y3, Y4, Y5, Y6, Y7, X2, Y10, Y11 peak in the finished tablet standard finger-print, totally 9 peaks; The characteristic peak of ownership Semen Cuscutae is T2, T3, T4, T5, T6 peak, totally 5 peaks; The characteristic peak of ownership Rhizoma Cibotii is G1, G2, G3, G4, G5, G6, G7, G8 peak, totally 8 peaks; The X1 peak is the stack peak at T1 peak in Y1 peak and the Semen Cuscutae standard finger-print in the intermediate extractum standard finger-print.
Second the step, measure epimedium herb to be measured with above-mentioned identical method, Semen Cuscutae medical material, Rhizoma Cibotii medical material, intermediate extractum, the finger printing of finished tablet.
The 3rd step, with the finger printing of epimedium herb to be measured and standard finger-print comparison, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is applied to production greater than 0.950 epimedium herb.
Finger printing and its standard finger-print of Semen Cuscutae medical material to be measured are compared, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is applied to production greater than 0.900 Semen Cuscutae medical material.
Finger printing and its standard finger-print of Rhizoma Cibotii medical material to be measured are compared, and software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is applied to production greater than 0.950 Rhizoma Cibotii medical material.
Finger printing and its standard finger-print of intermediate extractum to be measured are compared, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity enters next road production operation greater than 0.950 intermediate extractum.
Finger printing and its standard finger-print of finished tablet to be measured are compared, and software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is dispatched from the factory as certified products greater than 0.900 finished tablet.
In addition, need to prove: because fingerprint pattern technology does not also become national standard, so test and produce the national standard requirement that all will reach corresponding medical material in the pharmacopeia with Herba Epimedii, Semen Cuscutae, Rhizoma Cibotii, Fructus Rosae Laevigatae, Fructus Ligustri Lucidi medical material among the present invention, finished tablet will reach this drug standard requirement that my company ratifies through national correlation department.
Investigate through methodology, HPLC method of the present invention is detecting three flavor medical materials, and when intermediate extractum and finished tablet, its precision, stability, repeatability are all better.
Chromatographic fingerprinting is order, ratio and the mutual restriction relation of the chromatographic peak that will reflect in the chromatogram feature as test sample.Under identical chromatographic conditions, the finger printing of product to be tested and the standard finger-print of having set up relatively screen satisfactory product to be tested from the overall similarity of two figure.The finger printing of three flavor medical materials to be measured and standard finger-print comparison separately among the present invention, overall similarity is produced as raw material for satisfactory batch, the overall similarity of finger printing and its standard finger-print enters next process for satisfactory batch in the intermediate extractum to be measured, and the overall similarity of finger printing and its standard finger-print dispatches from the factory as certified products for satisfactory batch in the finished tablet to be measured.
Advantage of the present invention:
1, the invention provides a kind of method that detects kidney-tonifying body-strengthening tablet quality with fingerprint pattern technology.Utilization the present invention can effectively guarantee the stable, consistent of final drug quality, and stronger to the identification power of the medicine true and false, to the monitoring of drug quality with estimate more comprehensively, and the theory of also more compound Chinese medicine " monarch, minister, help, make " wholistic therapy.
2, the present invention is respectively at raw medicinal material, intermediate extractum, the finished tablet three phases has been set up standard finger-print, and pointed out the ownership of each characteristic peak in intermediate extractum and the finished tablet standard finger-print, between three standard finger-prints, set up contact, thereby can reflect the transfer case of each main component in drug production process in the Chinese crude drug intuitively.
3, the present invention has realized from medical material to intermediate extractum making the easier control of production technology to the omnidistance quality control method of finished product again, adjusts also more science, rationally, finally makes the quality of finished product reach stable.
4, the chromatographic fingerprinting of setting up with the present invention is done as a wholely to treat, pay attention to order, ratio and the mutual restriction relation of each characteristic peak, pay attention to global similarity.The one-sidedness of both having avoided only measuring one, two chemical constituent and having judged total quality, having reduced again is the probability of the artificial processing of requisite quality.
5, the present invention is easy, quick, stable, precision is high, good stability, be easy to grasp.
Description of drawings
Fig. 1 is an epimedium herb HPLC standard finger-print;
Fig. 2 is a Semen Cuscutae medical material HPLC standard finger-print;
Fig. 3 is a Rhizoma Cibotii medical material HPLC standard finger-print;
Fig. 4 is an intermediate extractum HPLC standard finger-print;
Fig. 5 is a BUSHEN QIANGSHEN PIAN finished tablet HPLC standard finger-print;
The specific embodiment
One, makes up the HPLC standard finger-print
1. instrument and reagent
1.1 instrument
Agilent 1100 chromatograph of liquid, the DAD detector; Shanghai must the SB5200 ultrasonic cleaner.
1.2 reagent
Methanol, analytical pure; Acetic acid, analytical pure; Acetonitrile, chromatographically pure, Di Ma company produces; Ultra-pure water, the WAHAHA pure water; The Rhizoma Cibotii medical material is produced in 10 batches of Gansu; The Semen Cuscutae medical material is produced in 10 batches of Inner Mongols; The Rhizoma Cibotii medical material is produced in 10 batches of Guangxi; 10 batches of intermediate extractum; 10 batches of finished tablets; 5 batches of Fructus Rosae Laevigatae medical materials; 5 batches of Fructus Ligustri Lucidi medical materials.
Above-mentioned Herba Epimedii, Semen Cuscutae, Rhizoma Cibotii, Fructus Rosae Laevigatae, Fructus Ligustri Lucidi medical material all reach the national standard requirement of corresponding medical material in the pharmacopeia after testing, and finished tablet reaches this drug standard requirement that my company ratifies through national correlation department.
2. chromatographic condition
Detect wavelength 350nm; Enlightening horse C18 post (200 * 4.6mm, 5 μ m); 30 ℃ of column temperatures; Flow velocity 1ml/min; Mobile phase is acetonitrile, 1% acetic acid solution, gradient elution, and the eluting ratio is:
T(min) CH3CN(％) 1％CH3COOH(％)
0 5 95
20 5 95
80 45 55
90 5 95
3. standard finger-print is set up
3.1 test liquid preparation:
1. take by weighing powder 2.0g in the epimedium herb, in tool plug conical flask, add 20ml 80% methanol solution, supersound extraction 60min is put coldly, filters, and gets subsequent filtrate and filters with 0.45 μ m microporous filter membrane, promptly gets the Herba Epimedii test liquid;
2. take by weighing powder 1.0g in the Semen Cuscutae medical material, other promptly get the Semen Cuscutae test liquid with 1.;
3. take by weighing powder 1.0g in the Rhizoma Cibotii medical material, other promptly get the Rhizoma Cibotii test liquid with 1.;
4. take by weighing intermediate extractum 0.6g, other promptly get intermediate extractum test liquid with 1.;
5. take by weighing BUSHEN QIANGSHEN PIAN finished product fine powder 3.0g, other are same 1., and the tablet test liquid gets product.
3.2 algoscopy: draw above-mentioned test liquid 20ul respectively and inject hplc determination, the chromatogram of record 90min.
3.3 the standard of structure fingerprint image: according to described method, 10 batches of epimedium herbs are produced in Gansu, 10 batches of Semen Cuscutae medical materials are produced in the Inner Mongol, 10 batches of Rhizoma Cibotii medical materials, 10 batches of intermediate extractum, 10 batches of finished tablets are produced in Guangxi, measure respectively, find out its common characteristic peak respectively, through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " match, set up HPLC standard colour chart finger printing separately.Be specially:
Shown in Figure 1, epimedium herb has selected 11 main common characteristic peaks altogether, is followed successively by the Y1-Y11 peak, and retention time is respectively: 31.8min, 47.4min, 53.8min, 59.0min, 59.7min, 60.4min, 61.7min, 63.3min, 66.8min, 78.6min, 83.0min.The relative standard deviation RSD% of described 11 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of epimedium herbs and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950.
Shown in Figure 2, the Semen Cuscutae medical material is selected 6 main common characteristic peaks altogether, is followed successively by the T1-T6 peak, and retention time is respectively: 31.8min, 44.3min, 46.2min, 46.7min, 50.1min, 68.4min.The relative standard deviation RSD% of described 6 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of Semen Cuscutae medical materials and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.900.
Shown in Figure 3, the Rhizoma Cibotii medical material is selected 8 main common characteristic peaks altogether, is followed successively by the G1-G8 peak, and retention time is respectively: 7.4min, 17.2min, 21.3min, 25.4min, 29.8min, 32.9min, 39.3min, 40.9min.The relative standard deviation RSD% of described 8 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of Rhizoma Cibotii medical materials and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950.
Shown in Figure 4, intermediate extractum method for making is that above-mentioned 10 batches of epimedium herbs become 10 batches of intermediate extractum with Fructus Rosae Laevigatae, Fructus Ligustri Lucidi medical material mixing decocting and concentrating respectively, and the weight ratio of every batch three flavor medical material is 161: 97: 97.Intermediate extractum is selected 11 main common characteristic peaks altogether, is Y1 successively, retention time 31.8min; Y2, retention time 47.4min; Y3, retention time 53.8min; Y4, retention time 59.0min; Y5, retention time 59.7min; Y6, retention time 60.4min; Y7, retention time 61.7min; X2, retention time 69.4min; Y10, retention time 78.6min; Y11, retention time 83.0min.The relative standard deviation RSD% of described 11 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of intermediate extractum and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950.
Shown in Figure 5, finished tablet is selected 23 main common characteristic peaks altogether, is successively: G1, retention time 7.4min; G2, retention time 17.2min; G3, retention time 21.3min; G4, retention time 25.4min; G5, retention time 29.8min; X1, retention time 31.8min; G6, retention time 32.9min; G7, retention time 39.3min; G8, retention time 40.9min; T2, retention time 44.3min; T3, retention time 46.2min; T4, retention time 46.7min; Y2, retention time 47.4min; T5, retention time 50.1min; Y3, retention time 53.8min; Y4, retention time 59.0min; Y5, retention time 59.7min; Y6, retention time 60.4min; Y7, retention time 61.7min; T6, retention time 68.4min; X2, retention time 69.5min; Y10, retention time 78.6min; Y11, retention time 83.0min.The relative standard deviation RSD% of described 23 peak retention times is all less than 1%.Overall similarity between the finger printing of 10 batches of finished tablets and its standard finger-print is through software---and " the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.900.
3.4 methodological study
3.4.1 precision is investigated
Respectively with same Herba Epimedii, Semen Cuscutae, Rhizoma Cibotii, intermediate extractum, finished tablet test liquid, continuous sample introduction 6 times is investigated the precision of instrument.With main component retention time and calculated by peak area, as a result retention time except the RSD at preceding 4 peaks of finished product 0.7-1.2%, the RSD at other peaks＜0.3%; Peak area changes than big the RSD at other peaks＜3% except the T6 peak in the Semen Cuscutae test liquid.The result shows that precision is good.
3.4.2 study on the stability
Respectively with same Herba Epimedii, Semen Cuscutae, Rhizoma Cibotii, intermediate extractum, finished tablet test liquid, 0,1.5h, 3h, 4.5h, 6h, the 24h sample introduction is investigated stability of sample.Investigate the same precision of index, as a result retention time except the RSD at preceding 4 peaks of finished product at 0.7-1.2%, the RSD at other peaks＜0.3%; Peak area is (prolonging peak area in time reduces) except the T6 peak changes greatly in the Semen Cuscutae test liquid, the RSD at other peaks＜3%.The result shows that test liquid is stable in 24h.
3.4.3 repeatability is investigated
In with a collection of Herba Epimedii, Semen Cuscutae, Rhizoma Cibotii, intermediate extractum, finished tablet, according to the sample preparation methods of having set up, repeat to extract 5 parts respectively, carrying out HPLC then analyzes, with the main component calculated by peak area, the results peaks area changes than big the RSD at other peaks＜4% except the T6 peak in the Semen Cuscutae test liquid.The result shows that the method repeatability is good.
Two, measure 5 batches of commercially available epimedium herbs to be measured (except that 10 batches that have adopted) respectively according to described detection method and condition, gather the 90min chromatogram, be these 5 batches epimedium herb finger printing to be measured.
Measure 2 batches of commercially available Semen Cuscutae medical materials to be measured (except that 10 batches that have adopted) respectively according to described detection method and condition, gather the 90min chromatogram, be these 2 batches Semen Cuscutae medicinal materials fingerprints to be measured.
Measure 2 batches of commercially available Rhizoma Cibotii medical materials to be measured (except that 10 batches that have adopted) respectively according to described detection method and condition, gather the 90min chromatogram, be these 2 batches Rhizoma Cibotii medicinal materials fingerprints to be measured.
Intermediate extractum when measuring 5 batches of production BUSHEN QIANGSHEN PIAN respectively according to described detection method and condition (except that 10 batches that have adopted) is gathered the 90min chromatogram, is these 5 batches intermediate extractum finger printing to be measured.
Measure 5 batches of BUSHEN QIANGSHEN PIAN finished tablets (except that 10 batches that have adopted) respectively according to described detection method and condition, gather the 90min chromatogram, be these 5 batches finished tablet finger printing to be measured.
Three, this medical material standard finger-print of setting up in 5 batches of epimedium herb finger printing to be measured and 3.3 is compared, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, similarity is respectively 0.983 as a result, 0.983,0.997,0.986,0.987.The similarity of the 5 batches of medical materials and standard finger-print is greater than 0.950, and meets simultaneously under the situation of epimedium herb standard in the pharmacopeia, can use aborning.
This medical material standard finger-print of setting up in 2 batches of Semen Cuscutae medicinal materials fingerprints to be measured and 3.3 is compared, and software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity, and similarity is respectively 0.962,0.812 as a result in employing.In the two batches of medical materials with the similarity of standard finger-print greater than 0.900 that is a collection of, and meet simultaneously under the situation of Semen Cuscutae medical material standard in the pharmacopeia, can use aborning.
This medical material standard finger-print of setting up in 2 batches of Rhizoma Cibotii medicinal materials fingerprints to be measured and 3.3 is compared, and software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity, and similarity is respectively 0.982,0.989 as a result in employing.The similarity of the two batches of medical materials and standard finger-print is greater than 0.950, and meets simultaneously under the situation of Rhizoma Cibotii medical material standard in the pharmacopeia, can use aborning.
The intermediate extractum standard finger-print of setting up in 5 batches of intermediate extractum finger printing to be measured and 3.3 is compared, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, similarity is respectively 0.998 as a result, 0.999,0.997,0.999,0.999.The similarity of the 5 batches of intermediate extractum and standard finger-print can enter next process greater than 0.950.
The finished tablet standard finger-print of setting up in 5 batches of finished tablet finger printing to be measured and 3.3 is compared, and software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity, and similarity is respectively 0.993 as a result in employing, 0.999,0.997,0.992,0.993.The similarity of the 5 batches of finished tablets and standard finger-print is greater than 0.900, and reaches my company simultaneously under the situation that this drug standard of national correlation department approval requires, and can be used as certified products and dispatches from the factory.
Claims (4)
1. one kind is detected the method for kidney-tonifying body-strengthening tablet quality with fingerprint pattern technology, comprises following content:
The first step, structure HPLC standard finger-print, method is as follows:
(a), test liquid preparation:
1. take by weighing powder 2.0g in the epimedium herb, in tool plug conical flask, add 20ml 80% methanol solution, supersound extraction 60min is put coldly, filters, and gets subsequent filtrate and filters with 0.45 μ m microporous filter membrane, promptly gets the Herba Epimedii test liquid;
2. take by weighing powder 1.0g in the Semen Cuscutae medical material, other promptly get the Semen Cuscutae test liquid with 1.;
3. take by weighing powder 1.0g in the Rhizoma Cibotii medical material, other promptly get the Rhizoma Cibotii test liquid with 1.;
4. take by weighing intermediate extractum 0.6g, other promptly get intermediate extractum test liquid with 1.;
5. take by weighing BUSHEN QIANGSHEN PIAN finished product fine powder 3.0g, other are same 1., and the tablet test liquid gets product;
(b), chromatographic condition: Agilent 1100 type high performance liquid chromatographs, the DAD detector detects wavelength 350nm; 200 * 4.6mm of enlightening horse, 5 μ m C18 posts; 30 ℃ of column temperatures; Flow velocity 1ml/min; Mobile phase is acetonitrile, 1% acetic acid solution, gradient elution, and the eluting ratio is:
T-min CH3CN％ 1％CH3COOH％
0 5 95
20 5 95
80 45 55
90 5 95
(c), algoscopy: draw above-mentioned test liquid 20ul respectively and inject hplc determination, the chromatogram of record 90min;
10 batches of epimedium herbs are produced in Gansu, 10 batches of Semen Cuscutae medical materials are produced in the Inner Mongol, 10 batches of Rhizoma Cibotii medical materials are produced in Guangxi, 10 batches of intermediate extractum, 10 batches of finished tablets are measured respectively, find out its main common characteristic peak respectively, through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " match, set up HPLC standard colour chart finger printing separately, be specially:
Epimedium herb has selected 11 main common characteristic peaks altogether, be followed successively by the Y1-Y11 peak, retention time is respectively: 31.8min, 47.4min, 53.8min, 59.0min, 59.7min, 60.4min, 61.7min, 63.3min, 66.8min, 78.6min, 83.0min, the relative standard deviation RSD% of described 11 peak retention times all less than the finger printing of 1%, 10 batch of epimedium herb and the overall similarity between its standard finger-print through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950;
The Semen Cuscutae medical material is selected 6 main common characteristic peaks altogether, be followed successively by the T1-T6 peak, retention time is respectively: 31.8min, 44.3min, 46.2min, 46.7min, 50.1min, 68.4min, the relative standard deviation RSD% of described 6 peak retention times all less than the finger printing of 1%, 10 batch of Semen Cuscutae medical material and the overall similarity between its standard finger-print through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.900;
The Rhizoma Cibotii medical material is selected 8 main common characteristic peaks altogether, be followed successively by the G1-G8 peak, retention time is respectively: 7.4min, 17.2min, 21.3min, 25.4min, 29.8min, 32.9min, 39.3min, 40.9min, the relative standard deviation RSD% of described 8 peak retention times all less than the finger printing of 1%, 10 batch of Rhizoma Cibotii medical material and the overall similarity between its standard finger-print through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950;
Intermediate extractum is selected 11 main common characteristic peaks altogether, is Y1 successively, retention time 31.8min; Y2, retention time 47.4min; Y3, retention time 53.8min; Y4, retention time 59.0min; Y5, retention time 59.7min; Y6, retention time 60.4min; Y7, retention time 61.7min; X2, retention time 69.4min; Y10, retention time 78.6min; Y11, retention time 83.0min, the relative standard deviation RSD% of described 11 peak retention times all less than the finger printing of 1%, 10 batch of intermediate extractum and the overall similarity between its standard finger-print through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.950;
Finished tablet is selected 23 main common characteristic peaks altogether, is successively: G1, retention time 7.4min; G2, retention time 17.2min; G3, retention time 21.3min; G4, retention time 25.4min; G5, retention time 29.8min; X1, retention time 31.8min; G6, retention time 32.9min; G7, retention time 39.3min; G8, retention time 40.9min; T2, retention time 44.3min; T3, retention time 46.2min; T4, retention time 46.7min; Y2, retention time 47.4min; T5, retention time 50.1min; Y3, retention time 53.8min; Y4, retention time 59.0min; Y5, retention time 59.7min; Y6, retention time 60.4min; Y7, retention time 61.7min; T6, retention time 68.4min; X2, retention time 69.5min; Y10, retention time 78.6min; Y11, retention time 83.0min, the relative standard deviation RSD% of described 23 peak retention times all less than the finger printing of 1%, 10 batch of finished tablet and the overall similarity between its standard finger-print through software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004A of system " calculates all greater than 0.900;
Second the step, measure epimedium herb to be measured with above-mentioned identical method, Semen Cuscutae medical material, Rhizoma Cibotii medical material, intermediate extractum, the finger printing of finished tablet;
The 3rd step, with the finger printing of epimedium herb to be measured and standard finger-print comparison, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is applied to production greater than 0.950 epimedium herb;
Finger printing and its standard finger-print of Semen Cuscutae medical material to be measured are compared, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is applied to production greater than 0.900 Semen Cuscutae medical material;
Finger printing and its standard finger-print of Rhizoma Cibotii medical material to be measured are compared, and software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is applied to production greater than 0.950 Rhizoma Cibotii medical material;
Finger printing and its standard finger-print of intermediate extractum to be measured are compared, software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity enters next road production operation greater than 0.950 intermediate extractum;
Finger printing and its standard finger-print of finished tablet to be measured are compared, and software---" the chromatographic fingerprints of Chinese materia medica similarity evaluation 2004B of system " calculates overall similarity in employing, and the screening similarity is dispatched from the factory as certified products greater than 0.90 finished tablet.
2. a kind of method that detects kidney-tonifying body-strengthening tablet quality with fingerprint pattern technology according to claim 1, it is characterized in that: intermediate extractum method for making is that 10 batches of epimedium herbs that make up the Herba Epimedii standard finger-print become 10 batches of intermediate extractum with Fructus Rosae Laevigatae, Fructus Ligustri Lucidi medical material mixing decocting and concentrating respectively, and the weight ratio of every batch three flavor medical material is 161: 97: 97.
3. a kind of method that detects kidney-tonifying body-strengthening tablet quality with fingerprint pattern technology according to claim 1, it is characterized in that: the characteristic peak of ownership Herba Epimedii is Y1, Y2, Y3, Y4, Y5, Y6, Y7, Y10, Y11 peak in the intermediate extractum standard finger-print, totally 9 peaks; The X2 peak is newly-increased composition.
4. a kind of method that detects kidney-tonifying body-strengthening tablet quality with fingerprint pattern technology according to claim 1, it is characterized in that: the characteristic peak of ownership intermediate extractum is Y2, Y3, Y4, Y5, Y6, Y7, X2, Y10, Y11 peak in the finished tablet standard finger-print, totally 9 peaks; The characteristic peak of ownership Semen Cuscutae is T2, T3, T4, T5, T6 peak, totally 5 peaks; The characteristic peak of ownership Rhizoma Cibotii is G1, G2, G3, G4, G5, G6, G7, G8 peak, totally 8 peaks; The X1 peak is the stack peak at T1 peak in Y1 peak and the Semen Cuscutae standard finger-print in the intermediate extractum standard finger-print.
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| CN103257191B (en) * | 2013-04-27 | 2015-02-25 | 太极集团重庆涪陵制药厂有限公司 | Method for assaying kidney tonifying and life lengthening capsule fingerprint |
| CN105606752A (en) * | 2016-01-22 | 2016-05-25 | 哈尔滨市康隆药业有限责任公司 | Detection method of fingerprint spectrums of sugar-free strong pipa syrup |
| CN106153805B (en) * | 2016-08-29 | 2017-11-28 | 山东大学 | A kind of construction method of analgesic capsule of corydalis tuber finger-print and its application |
| CN110441441B (en) * | 2019-09-20 | 2022-03-29 | 广东一方制药有限公司 | UPLC characteristic spectrum construction method and identification method of rhizoma cibotii and rhizoma cibotii scalding medicinal materials |
| CN110501445B (en) * | 2019-09-30 | 2020-12-01 | 青岛琛蓝医药科技发展有限公司 | Quality control and fingerprint spectrum detection method for epimedium compound |
| CN111337448B (en) * | 2020-03-26 | 2023-05-12 | 杭州老爸评测科技股份有限公司 | Method for identifying cosmetics based on infrared spectrum technology |
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| CN1364531A (en) * | 2001-01-11 | 2002-08-21 | 杨孟君 | Nano kidney tonifying and body strengthening medicine and its preparing method |
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| CN1365808A (en) * | 2001-01-18 | 2002-08-28 | 杨孟君 | Nano medicine 'Guilu Bushen' and its preparing process |
| CN1895401A (en) * | 2006-06-26 | 2007-01-17 | 河南康鑫药业有限公司 | Preparation of kidney-tonifying health-care tablet by micropowder technology |
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