超高效液相色谱-串联质谱法同时测定动物组织中4种抗结核药物的残留量

Ultra performance liquid chromatography-tandem mass spectrometry for simultaneous determination of four antituberculosis agents residues in animal tissue

建立了超高效液相色谱-串联质谱法同时测定鸡肉、牛肉、猪肉中4种抗结核药物残留量的检测方法。样品经酸化乙腈超声提取,HLB固相萃取柱净化,LunaC8柱(150 mm×2 mm,3μm)分离,电喷雾电离(ESI^+)和多反应监测(MRM)模式检测。结果表明,利福平、利福霉素、利福喷汀和利福布汀分别在0.3"20.0,0.1"20.0,0.3"20.0,0.2"20.0μg/L范围内呈良好线性,相关系数大于0.99,定量限为0.8"1.2μg/kg。在1.0,2.0,10.0μg/kg添加水平的平均回收率为66.3%~104.5%,日内相对标准偏差为4.2%~13.8%(n=6),鸡肉的日间相对标准偏差为4.3%~13.6%(n=3)。该法可用于动物组织中4种抗结核药物残留量的同时检测。

A method for simultaneous determination of four antituberculosis agent residues in animal tissue by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)wasestablished.The samples were ultrasonically extracted with acidified acetonitrile,and purified by HLB column.Subsequently,the target compounds were separated by Luna■C8 column(150mm×2mm,3μm),and determined by mass spectrometry with electrospray ion source under the positive and multiple-reaction monitoring(MRM)modes.The linear ranges of rifampin,rifamycin,rifapentine and rifabutin were 0.3-20.0,0.1-20.0,0.3-20.0,0.2-20.0μg/L,respectively,with the correlation coefficients(R2)ofabove 0.99.The limits of quantitation(LOQs)of the four antituberculosis agent residues were in the range of 0.8-1.2μg/kg.At the spiked levels of 1.0,2.0 and10.0μg/kg,the average recoveries of the four antituberculosis agent residues were from 66.3%to 104.5%,and the intra day relative standard deviations were 4.2%-13.8%(n=6),the inter day relative standard deviations of chicken were 4.3%-13.6%(n=3).The results indicated that the method is suitable tosimultaneously determine the four antituberculosis agent residues in animal tissue.