LC-MS/MS同时测定一清胶囊9个成分的含量

目的: 建立运用液相色谱-串联质谱法同时测定一清胶囊中9个成分(黄芩苷、汉黄芩苷、黄连碱、药根碱、巴马汀、小檗碱、大黄素、大黄酚、大黄素甲醚)含量的分析方法。 方法: 采用Agilent SB-C₁₈色谱柱(2.1 mm×50 mm,1.8 μm),以水-甲醇为流动相,梯度洗脱(0~4.5 min,20%B→70%B;4.5~8 min,70%B→95%B;8~8.5 min,95%B→20%B),流速0.3 mL·min^-1,柱温为室温;采用电喷雾离子源(ESI),动态多反应监测扫描模式(DynamicMRM)进行定量分析,干燥气温度350℃,干燥气流量10 L·min^-1,雾化器压力275.8 kPa,毛细管电压4 kV。 结果: 黄芩苷、汉黄芩苷、黄连碱、药根碱、巴马汀、小檗碱、大黄素、大黄酚、大黄素甲醚的质量浓度分别在2.712~27.12 μg·mL^-1(r=0.9989)、0.8800~8.800 μg·mL^-1(r=0.9991)、0.5280~5.280 μg·mL^-1(r=0.9982)、0.1272~1.272 μg·mL^-1(r=0.9977)、0.3024~3.024 μg·mL^-1(r=0.9979)、1.196~11.96 μg·mL^-1(r=0.9995)、33.28~332.8 ng·mL^-1(r=0.9988)、32.40~324.0 ng·mL^-1(r=0.9974)、8.800~88.00 ng·mL^-1(r=0.9977);平均加样回收率(n=6)均在97.5%~101.9%范围内,RSD均小于2.4%。 结论: 该分析方法特异、快速、灵敏,重复性好,可为一清胶囊的质量控制提供依据。

Objective: To establish an LC-MS/MS method for simultaneous content determination of the nine components (baicalin,wogonoside, coptisine, jatrorrhizine, palmatine, berberine, emodin, chrysophanol, physcion) in Yiqing capsules. Methods: The HPLC analysis was performed on an Agilent SB-C₁₈ column (2.1 mm×50 mm,1.8 μm) with gradient elution using water and methanol as the mobile phase (0-4.5 min, 20%B→70%B; 4.5-8 min, 70%B→95%B; 8-8.5 min, 95%B→20%B). The flow rate was 0.3 mL·min^-1, the column temperature was room temperature. Electrospray ionization(ESI) source was used. Quantization was performed using selected dynamic multiple reaction monitoring (DynamicMRM) mode(gas tempereture:350℃; gas flow:10 L·min^-1; nebulizer:275.8 kPa; capillary:4 kV). Results: The method has a good linearity in the ranges of 2.712-27.12 μg·mL^-1(r=0.9989) for baicalin, 0.8800-8.800 μg·mL^-1(r=0.9991) for wogonoside, 0.528-5.280 μg·mL^-1(r=0.9982) for coptisine, 0.1272-1.270 μg·mL^-1(r=0.9977) for jatrorrhizine, 0.3024-3.024 μg·mL^-1(r=0.9979) for palmatine, 1.196-11.96 μg·mL^-1(r=0.9995) for berberine, 33.28-332.8 ng·mL^-1(r=0.9988) for emodin, 32.40-324.0 ng·mL^-1(r=0.9974) for chrysophanol, 8.800-88.00 ng·mL^-1(r=0.9977) for physcion.The average recoveries of nine active components were 97.5%-101.9% with RSDs (n=6) of less than 2.4%. Conclusion: The method is specific, rapid, sensitive and reliable. It may provide a basis for the quality control of Yiqing capsules.