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Objective To develop a new method to determine the contents of rutaecarpine in Fuzhengpingxiao capsule by HPLC method.Methods Samples were handled by ethanol and extraction with ethyl acetate.The separation was achieved on an Agilent TC-C18column using a mobile phase system of acetonitrile-water(2% Tetrahydrofuran and 0.2 % formic acid)at a flow rate of 1.0 ml/min.The temperature of column was 40 ℃ and the detection wavelength was 240 nm.Results The cali-bration curves of rutaecarpine showed good linearity in the ranges of 1.18-118 μg/ml,r=0.999 9.The results of intra-day and inter-day precisions were both within 2%,the average additional recovery rate was 94.20%.Conclusion The HPLC method was accurate,specific,sensitive and reproducible,which could be used for quality control of rutaecarpine in the preparation of Fuzhengpingxiao capsule.
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Objective To determine the content of paeoniflorin in Fuzhengpingxiao capsule by HPLC method .Methods The content of paeoniflorin were determined by HPLC ,and the column was an Agilent Zorbax SB-C18 column (150 mm × 4 .6 mm ,5 μm);The mobile phase was acetonitrile and 5 mmol/L sodium dihydrogen phosphate (10:90) ,and the flow rate was set at 1 ml/min .Column temperature was 25°C ,detection wavelength was 230 nm ,injection volume was 10 μl ,and running time was 25 min .Results Paeoniflorin was linear (r=0 .9999) in the concentration of 25 .0-500 .0 μg/ml ,the linear equation was Y=12 .65 X +43 .54 ,and the average recovery was 92 .69％ with RSD value was 1 .77％ .Conclusion The method was easy to operate ,reliable and reproducible ,which could be used in the determination of paeoniflorin in FuzhengPingxiao capsule .
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Objective To use high-performance liquid chromatography-time of flight mass spectrometry (HPLC-TOF/ MS) for analyzing the chemical constituents of Fuzhengpingxiao Capsule. Methods The separation was performed on a Agilent Eclipse plus C18 reverse phase column (4. 6 mm×250 mm, 5 μm). The mobile phase consisted of water containing 0. 1% formic acid and acetonitrile was used as gradient elute. The flow rate was 1 ml/min, the post-column split ratio was 3:1, and the temperature of column was 25°C. Time-of-flight mass spectrometer(TOF/MS) and electrospray ion source (ESI) was employed for qualitative analysis under both positive and negative ion mode, and mass scan range was m/z 100-1 100. Results A total of 247 major chemical constituents were identified in Fuzhengpingxiao Capsule by HPLC-TOF/MS, including 168 in positive mode, 103 in negative mode, and 24 in both. The source herb of the components were identified. Conclusion An efficient HPLC-TOF/MS approach has been established for studying the chemical constituents in Fuzhengpingxiao Capsule, which paves a way for the quality control and further in vivo studies of the preparation.
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Objective: To establish a HPLC-MS method to simultaneously determine the contents of gentiopicroside, liquiritin, rosmarinic acid and harpagoside in Fuzhengpingxiao capsule. Methods The chromatographic separation was performed on a Agilent Eclipse plus C18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of acetonitrile (A)-0.1% methanoic acid (B) (0-30 min, 15% A-40% A), eluted at a flow rate of 1.0 ml/min and with a split ratio of 3: 1. Negative ionization and selected ion monitoring (SIM) mode on Mass were selected. Results The limit of quantitation (LOQ) values of gentiopicroside, liquiritin, rosmarinic acid and harpagoside were 5.73, 6.37, 6.50, and 6.46 ng/ml, and the limit of detection (LOD) values were 0.46, 0.32, 0. 33 and 0.32 ng/ml, respectively. Good linearity (r > 0.999 0) was obtained over the investigated concentration ranges. Reproducibility was evaluated by intra- and inter-day assays, and RSD values were below 2%. The average recoveries of the 4 compounds were within the range of 98%-102%. Conclusion We have established a rapid and efficient HPLC-MS method for determination of 4 constituents in Fuzheng pingxiao capsule: gentiopicroside, liquiritin, rosmarinic acid and harpagoside.