UPLC-MS/MS检测伤痛宁片中5个马兜铃酸成分

Determination of Five Aristolochic Acid Components in Shangtongning Tablets by Ultra-high Performance Liquid Chromatography-mass Spectrometry

目的:测定伤痛宁片中马兜铃酸类成分的含量。方法:采用超高效液相色谱-质谱法测定伤痛宁片中马兜铃酸Ⅰ、马兜铃酸Ⅱ、马兜铃酸Ⅲa、马兜铃酸AA-Ⅳa、马兜铃内酰胺Ⅰ的含量。采用Agilentporoshell C18(100 mm×2.1 mm,2.7μm)色谱柱,以乙腈(A)-0.1%甲酸水溶液(B)为流动相梯度洗脱;电喷雾正离子模式,多反应监测,进样量为1μL,以基质标准曲线外标法计算伤痛宁片中5个马兜铃酸成分含量。结果:18批样品中检出马兜铃酸Ⅰ质量分数为0.01~0.05 mg·kg^(–1),马兜铃酸Ⅱ和马兜铃酸Ⅲa未检出,马兜铃酸AA-Ⅳa质量分数为0.26~1.00 mg·kg^(–1),马兜铃内酰胺Ⅰ质量分数为0.40~2.17 mg·kg^(–1)。结论:建立的含量测定方法,可为伤痛宁片及含马兜铃酸中药制剂的临床应用和安全监管提供参考。

Objective:To determine the contents of aristolochic acid components in Shangtongning Tablets.Method:The contents of aristolochic acidⅠ,aristolochic acidⅡ,aristolochic acidⅢa,aristolochic acid AA-Ⅳa,and aristolochic lactamⅠin Shangtongning Tablets were determined by ultra-high performance liquid chromatography-mass spectrometry.Agilentporoshell C18 chromatographic column(100 mm×2.1 mm,2.7μm)was used,with acetonitrile(A)-0.1%formic acid solution(B)as mobile phase for gradient elution.Under Electrospray positive ion mode(ESI+)and multi-reaction monitoring(MRM)mode,the sample injection volume was 1μL,and the contents of five aristolochic acid components in Shangtongning Tablets were calculated using the matrix standard curve external standard method.Results:The contents of aristolochic acidⅠ,aristolochic acid AAⅣa,and aristolochic lactamⅠwere 0.01-0.05,0.26-1.00 and 0.40-2.17 mg·kg^(–1),respectively,in 18 batches of samples,with aristolochic acidⅡand aristolochic acidⅢa not detected.Conclusion:The content determination method established in this study can provide a reference for the clinical application and safety supervision of Shangtongning Tablets and traditional Chinese medicine preparations containing aristolochic acids.