The Quality Study Of Standard Preparation Of Fufang Danshen Tablets

Fufang Danshen tablets has been collected by China pharmacopoeia(ChP) as anational essential drug.The method of TLC analysis was established with three chromatographic systems toidentify the known or the unknown composition. The method of GC analysis wasestablished to control the content of borneol of Fufang Danshen tablet. The method offingerprint of HPLC analysis was established to resolve quality control of Fufang Danshentablet with active ingredients unclear and quality differences in different batches, at thesame time determine the content of part of compounds of Fufang Danshen tablets at thesame time. The study established UPLC methods to control the internal quality of FufangDanshen tablets quickly.In this TLC methods study, the samples was extracted by aether and70%(volumefraction) methanol water solution, the samples and standards were loaded on a TLC plate.After the TLC plate developing in the solvent system of toluene-ethyl acetate(19:1) andcoating of a slight2%(volume fraction) vanillin H2SO4,Salvia miltiorrhizae, Panaxnotoginseng and borneol were monitored at the same time. After the TLC plate developingin the solvent system of cyclohexane-ethyl acetate-methanol(5:2:1) and coating of a slight10%(volume fraction) H2SO4ethanol,the spots of cryptotanshinone, tanshinone Ⅰ,tanshinone ⅡA were clear and separated well. After the TLC plate developing in thesolvent system of dichloromethane-pure alcohol-water(70:45:6.5) and coating of a slight10%(volume fraction) H2SO4ethanol, the spots of ginsenoside Rb1,ginsenoside Rg1,ginsenoside Re,notoginsenoside R1were clear and separated well. The separating degree ofginsenoside Re and notoginsenoside R1were good. This method identify22the known orthe unknown characteristic spots of Fufang Danshen tablets through three silica gel60 plates. The method is rapid, simple, and suitable for the internal quality control of FufangDanshen tablets.The study used DB-WAX capillary column（30m×0.32mm×0.25μm）to establish GCmethods for determination of borneol in Fufang Danshen tablets. The determinetion ofborneol as follows: the temperature of column was110℃, the temperature of injection portwas200℃，the temperature of detector was200℃. The isoborneol standard curve waslinear in the rage of0.048-0.954mg/ml and the borneol standard curve was linear in therage of0.073-1.468mg/ml (r=0.999). The recovery of isoborneol was97.6%and therecovery of borneol was98.9%(n=6). There were large differences of the content ofborneol in various batches and various manufacturers of Fufang Danshen tablets. Themethod is rapid, simple, and suitable for the analysis of borneol in Fufang Danshen tablets.There are only the content limit of Sal B and tanshinone ⅡA,but non-salvianic acidA sodium, protocatechualdehyde, rosmarinic acid, cryptotanshinone, Tanshinone I blankunder HPLC chromatography in2010edition "Chinese Pharmacopoeia". The studyestablished HPLC fingerprint chromatogram of Fufang Danshen tablets. The separation wasperformed on Thermo ODS-2Hypersi（l250mm×4.6mm，5μm）columnn with mobile phaseconsisted of acetonitrile-0.1%formic acid（gradient elution）at flow rate of1.0ml/min.Detection wavelength was set at270nm and column temperature was30℃.15copossessing peaks were selected as the fingerprint peaks by analyzing10batches ofFufang Danshen tablets. At the same time, we examined the content of salvianic acid Asodium, protocatechualdehyde, rosmarinic acid, cryptotanshinone, TanshinoneI,tanshinoneIIA. The method is rapid, simple, repeatable and suitable for the internalquality control of Fufang Danshen tablets.The study established UPLC methods of Fufang Danshen tablets. The separation wasperformed on ACQUITY UPLC BEH C-18（1.7μm2.1×50mm）columnn with mobilephase consisted of acetonitrile-water（gradient elution）at flow rate of0.2ml/min. Detectionwavelength was set at203nm and column temperature was30℃. The content of foursaponins in Fufang Danshen tablets among10batches from the same manufacturer is morethan6.0mg per pill．There is great variability in the content of four saponins in Fufang Danshen tablets from10different manufacturers. The method is rapid, simple, repeatableand suitable for the internal quality control of Fufang Danshen tablets quickly.