快速液相色谱-串联质谱联用同时检测抗风湿类中药制剂中13种添加化学药物成分

目的: 建立快速液相-串联质谱方法检测中药制剂中添加13种化学药物成分(氨基比林、对乙酰氨基酚、甲氧苄啶、阿司匹林、氢化可的松、吡罗昔康、醋酸泼尼松、萘普生、地塞米松、双氯芬酸钠、吲哚美辛、布洛芬、保泰松)。 方法: 采用Agilent Eclipse Plus C₁₈色谱柱(2.1 mm×100 mm,1.8 μm);梯度洗脱:流动相A为0.1%甲酸水溶液,流动相B为乙腈。通过比较样品峰与对照品峰的保留时间、一级质谱和二级质谱碎片离子,确定样品中是否掺杂化学抗风湿药物。 结果: 建立的快速液相-串联质谱方法检测上述化学药物成分不受药物辅料干扰,各色谱峰分离良好,13种待测成分最小检出限为0.0031~0.9471 ng。 结论: 该方法简便、准确、灵敏度高,可快速有效地判断中药制剂中是否非法掺入上述化学药品。

Objective: To develop a method for simultaneous determination of 13 chemicals added illegally in anti-rheumatic traditional Chinese medicines (TCMs) by rapid resolution liquid chromatography coupled with tandem mass spectrometry (RRLC-MS/MS). Methods: Separation was performed on Agilent Eclipse Plus C₁₈(2.1 mm×10 mm:1.8 μm) column by gradient elution with acetonitrile and 0.1% formic acid aqueous solution as the mobile phase. The chemicals detected in samples were identified by comparison of sample peaks with the retention time, mass spectra and the product ions with those of reference substances. Results: The developed RRLC-MS/MS method was interfered by the adjuvants. The peaks detected could be separated from each other. The range of detection limits (LODs) for 13 chemicals was 0.0031-0.9471 ng. Conclusion: The developed RRLC-MS/MS method was not convenient, accurate and sensitive, which could be used for rapid screening of above-mentioned chemicals added illegally in TCMs.