液相色谱-串联质谱法测定鸡肉和鸡蛋中3种硝基咪唑类药物

Determination of 3 kinds of nitroimidazoles in chicken and egg by liquid chromatography-tandem mass spectrometry

中文关键词:  硝基咪唑类药物  液相色谱-串联质谱法  前处理  测定方法

英文关键词:nitroimidazoles  liquid chromatography-tandem mass spectrometry  pretreatment  determination method

中文摘要:

      目的 优化液相色谱-串联质谱法测定鸡肉及鸡蛋样品中地美硝唑(dimetridazole, DMZ)、甲硝唑(metronidazole, MNZ)、替硝唑(tinidazole, TDZ)3种硝基咪唑类药物。方法 样品经过乙酸乙酯提取, 氮吹浓缩, 盐酸水溶液复溶, 正己烷除脂, 固相萃取柱净化, 以乙腈-0.1%乙酸水溶液为流动相, SB-Aq色谱柱分离, 液相色谱串联质谱法在多重反应监测(multiple reaction monitoring, MRM)正离子模式下检测, 外标法定量。结果 鸡肉、鸡蛋标准曲线在1~500 μg/kg的浓度范围内线性关系良好, 相关系数r>0.999, 方法的回收率在67.56%~97.91%之间, 相对标准偏差为0.90%~16.27%, 定量限(S/N=10)为5 μg/kg, 检出限(S/N=3)为1 μg/kg。结论 本方法样品前处理简单, 精密度、重复性和回收率较好, 适用于批量测定鸡肉及鸡蛋样品中3种硝基咪唑类药物。

英文摘要:

      Objective To optimize the pretreatment method and detection conditions for the determination of 3 kinds of nitroimidazoles including nitroimidazoles, dimetridazole (DMZ), metronidazole (MNZ), tinidazole (TDZ) in chicken and egg by liquid chromatography-tandem mass spectrometry. Methods The sample was extracted with ethyl acetate, concentrated by nitrogen blowing, reconstituted with aqueous hydrochloric acid, degreased with n-hexane, purified by solid phase extraction column, separated by acetonitrile-0.1% acetic acid aqueous solution and SB-Aq column, tested by liquid chromatography tandem mass spectrometry in multiple reaction monitoring (MRM) positive ion mode and quantified by external standard method. Results Chicken and egg samples standard curve had good linear relationships in the range of 1?500 μg/kg, with the correlation coefficients were larger than 0.999. The recoveries were 67.56%?97.91%, with the relative standard deviations (RSDs) of 0.90%?16.27%. The limits of detection (LOD) and the limits of quantitation ((LOQ) were 1 and 5 μg/kg, respectively. Conclusion This method is simple in sample pretreatment, good in precision, repeatability and recovery, which is suitable for batch determination of 3 nitroimidazole drugs in chicken and egg samples