首页|UPLC-MS/MS检测伤痛宁片中5个马兜铃酸成分

UPLC-MS/MS检测伤痛宁片中5个马兜铃酸成分

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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,2.7 μm)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 1 μL,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.
Determination of Five Aristolochic Acid Components in Shangtongning Tablets by Ultra-high Performance Liquid Chromatography-mass Spectrometry
Objective:To determine the contents of aristolochic acid components in Shangtongning Tablets.Method:The contents of aristolochic acid Ⅰ,aristolochic acid Ⅱ,aristolochic acid Ⅲa,aristolochic acid AA-Ⅳa,and aristolochic lactam Ⅰ in Shangtongning Tablets were determined by ultra-high performance liquid chromatography-mass spectrometry.Agilentporoshell C18 chromatographic column(100 mm×2.1 mm,2.7 μm)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 1 μL,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 acid Ⅰ,aristolochic acid AA Ⅳa,and aristolochic lactam Ⅰ were 0.01-0.05,0.26-1.00 and 0.40-2.17 mg·kg-1,respectively,in 18 batches of samples,with aristolochic acid Ⅱ and aristolochic acid Ⅲa 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.

Shangtongning Tabletsaristolochic acidsaristolochic acid Ⅰaristolochic acid Ⅱquality control

张万青、陈佩文、刘潇潇、戴忠

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广东省药品检验所 广东省药品监督管理局中药质量控制与安全评价重点实验室,广东 广州 510663

中国食品药品检定研究院,北京 100050

伤痛宁片 马兜铃酸 马兜铃酸Ⅰ 马兜铃酸Ⅱ 质量控制

广东省药品监督管理局科技创新项目广东省医学科研基金项目

2023YDZ03B2023258

2024

中国现代中药
中国中药协会,中国医药集团总公司,中国药材公司

中国现代中药

CSTPCD
影响因子:0.65
ISSN:1673-4890
年,卷(期):2024.26(8)