Study On Quality Control Of Compound Shiwei Tablets

As an extension of the development of traditional Chinese medicine,traditional Chinese medicine compound preparation is a commonly used drug for the prevention and treatment of diseases.To improve the quality standards of traditional Chinese medicine compound preparations,improve the quality control methods of traditional Chinese medicine compound preparations,and comprehensively improve the overall quality control level of traditional Chinese medicine compound preparations,thereby contributing to the improvement of the safety and efficacy of traditional Chinese medicine compound preparations.Compound Shiwei Tablet is a traditional Chinese medicine compound preparation consisting of Astragalus membranaceus(Fisch.)Bunge.,Pyrrosia lingua(Thunb.)Farwell,Sophora flavescens and Polygonumaviculare L.It is produced exclusively by Jingfukang Pharmaceutical Group Co.,Ltd.In the 2015 edition of "Chinese Pharmacopoeia",it has the functions of clearing heat and dampness,diuretic and drenching,and is used for hot shower caused by damp heat.It is unfavorable for urinary tract caused by acute glomerulonephritis,pyelonephritis,cystitis and urethritis.The effects of edema,frequent urination,urgency,and dysuria are obvious.Compound Shiwei tablets are very popular among clinicians because of their unique curative effect,and have good market prospects.In the current standard of Compound Shiwei tablets,qualitative identification of quercetin in chlorogenic acid and scutellaria in Shiwei is determined by the content of astragaloside in Astragalus membranaceus and matrine in Sophora flavescens.The chemical composition of traditional Chinese medicine compound preparation is complicated.Although the determination of single component content plays a certain role in quality control,it cannot comprehensively evaluate the quality of traditional Chinese medicine compound preparation.As a multi-index comprehensive evaluation quality control model,fingerprints can be used to qualitatively and quantitatively analyze the chemical constituents in traditional Chinese medicine compound preparations.Therefore,this study further increases and improves the quality control methods of Compound Shiwei tablets.The content of the determination,the fingerprint of the Compound Shiwei tablets was established to control its quality comprehensively.The determination method of the content of astragaloside I,astragaloside II and astragaloside IV in Compound Shiwei tablets was established,and the fingerprint method and saponin were established.The method of containing samples was applied to the quality control of the Compound Shiwei tablet during the production process to investigate the mass transfer in the production process.This study also made a preliminary exploration of the method for determining the content of flavonoids in Compound Shiwei tablets.It is important to achieve complete control of the formulation process.preparation process.Objective:1 The fingerprint method of Compound Shiwei tablets was established by HPLC method,and the quality control of the preparation process was carried out to provide a basis for comprehensive control of the quality of Compound Shiwei tablets.2 HPLC-ELSD method was used to establish the determination methods of three kinds of saponins in Compound Shiwei tablets: astragaloside I,astragaloside II and astragaloside IV,and to investigate the three saponin components in the Compound Shiwei tablet preparation process.The quality of the transfer,multi-indicators control its quality,improve and improve the quality control method of Compound Shiwei tablets.3 Simultaneous determination of four flavonoids from ononin,calycosin-7-glucoside,calycosin,and formononetin in Compound Shiwei Tablets by HPLC was carried out to further study the control of Compound Shiwei tablets.The quality of the flavonoids provides the basis for the test.Methods:1 An Agilent 5 TC C18(2)column(250 mm × 4.6 mm,5 ?m)was used with a mobile phase of acetonitrile(A)-0.2% phosphoric acid(B)solution with a gradient elution(0~30~45~90min,phase A is 3%~11%~16%~30%),volume flow is 1.0 m L/min,detection wavelength: 235 nm,column temperature: 25 °C,injection volume: 10 ?L,for Compound Shiwei tablets And its intermediate(extract,granule)samples were measured.2 High-performance liquid chromatography-evaporative photodetector using an Agilent 5-HC C18(2)column(250 mm × 4.6 mm,5 ?m)with a mobile phase of acetonitrile(A)-water(B)for gradient washing Degassing(0~30~60~80~85min,phase A is 30%~33%~45%~80%~30%),flow rate 1.0 m L/min,column temperature 30 °C,injection volume 20 ?L.ELSD parameters: carrier gas flow rate of 1.5 L/min;Drift tube temperature of 90 °C,and determination of the content of astragalus saponin I,astragaloside II and astragaloside IV in the finished product,granule and extract sample of Astragalus membranaceus and Compound Shiwei tablets,And investigate the mass transfer of these three saponins in the preparation process of Compound Shiwei tablets3 By examining different chromatographic conditions,different extraction methods and other experimental studies,the HPLC method was used to simultaneously determine the content of four flavonoids in Compound Shiwei tablets: Ononin,Calycosin-7-glucoside,Calycosin,and formononetin.Results:1 Fingerprints of 14 batches of different batches of Compound Shiwei tablets and 3 batches of Compound Shiwei tablets intermediates(extracts,granules)were determined,and 14 batches of Compound Shiwei tablets were passed through the Chinese Traditional Medicine Chromatographic Fingerprint Similarity Evaluation System(2012 edition).The similarity evaluation was carried out on the fingerprint of Wei tablets.The common pattern of HPLC fingerprint of Compound Shiwei tablets was obtained.18 common peaks were identified,and 5 peaks were identified.The RSD values of common peak relative retention times of each batch were obtained <0.3%,similarity between batches > 0.990.The similarity between the same batch of Compound Shiwei tablet intermediate(extract,granule)and its finished product was >0.990,and the correlation was good.2 A method for the determination of astragaloside I,astragaloside II and astragaloside IV in Compound Shiwei tablets was established.Under these conditions,all three components reached baseline separation.The linear range of xanthine saponin I was 20.48~655.38?g/m L(r=0.9987),the average recovery rate was 99.58%,the RSD value was 2.95%;the linear range of xanthine saponin II was 21.44~686.00?g/m L(r=0.9994),the average recovery rate was 99.31%,and the RSD value was 2.48.%;the linear range of astragaloside IV was 16.74.44~535.57?g/m L(r=0.9997),the average recovery rate was 99.51%,and the RSD value was 2.46%.3 Through HPLC method,in the process of detecting four kinds of flavonoids in Compound Shiwei tablets: ononin,calycosin-7-glucoside,calycosin,and formononetin,after different extraction methods and chromatographic conditions,The chromatographic peak resolution of the sample is up to standard,but there is interference in the chromatogram of the negative sample,which needs further investigation and optimization.Conclution:1 The established HPLC method of Compound Shiwei Tablets is simple,effective and reproducible,and can be applied to the quality control of intermediates in the preparation process.The quality of Compound Shiwei tablets is evaluated for the first time.2 The established HPLC-ELSD method for the determination of the content of astragaloside I,astragaloside II and astragaloside IV in Compound Shiwei tablets is accurate,stable,simple,feasible and specific.It can also be used to investigate the process of Compound Shiwei tablets.The mass transfer of the three saponins in the body and Astragalus membranaceus has improved the quality control method of the Compound Shiwei tablets.4 The HPLC method was used to determine the content of f ononin,calycosin-7-glucoside,calycosin,and formononetin in Compound Shiwei tablets.The chromatographic peak resolution of the samples reached the standard,but the negative control map had interference.It is possible to establish a method for determining its content,which requires further research and exploration.