液相色谱-串联质谱同时监测猪尿中10种违禁药物

Simultaneous Determination of Ten Banned Substances in Pig Urine by Liquid Chromatography-Tandem Mass Spectrometry

建立了简单、灵敏、可靠的液相色谱-串联质谱测定猪尿中玉米赤霉醇及其类似物、氯霉素、五氯苯酚等10种违禁物质的分析方法。猪尿样品分别采用冻干法和Qu ECh ERS法前处理,乙腈和5 mmol/L乙酸铵溶液作为流动相,梯度洗脱,分析物经Zorbax SB-C18色谱柱分离,在电喷雾负离子模式下,采用四极杆质谱仪进行多反应监测分析。在实验浓度范围内,10种分析物基质匹配标准曲线线性良好,相关系数(R2)均大于0.99;在5、10及20μg/L添加浓度水平,两种前处理方法所得10种分析物的回收率分别为80.7%~107.7%和73.5%~103.3%,相对标准偏差均低于15%,检出限和定量限分别为0.1~2.0μg/L和0.2~5.0μg/L。本方法可满足生猪体内多种违禁物质的快速筛查监测要求。

A simple,sensitive and reliable method was developed for simultaneous determination of ten banned drugs residues including zeranols(ZALs),chloroamphenicol,pentachlorophenol,etc.in swine urine using liquid chromatography-tandem mass spectrometry(LC-MS/MS).The urine samples were pretreated using lyophilization and QuEChERS procedures,respectively.Acetonitrile and ammonium acetate(5 mmol/L)were chosen as mobile phases.Target compounds were separated well in ZorbaxSB-C 18 by following the optimized gradient elution program and determined by LC-MS/MS in negative electrospray ionization mode.The linearity of the matrix-matched standard curve of ten analytes in two methods was good in the range of the experimental concentration with correlation coefficients more than 0.99.The recoveries of ten drugs were in the range of 80.7%-107.7%and 73.5%-103.3%at the spiked levels of 5,10 and 20μg/L by lyophilization and QuEChERS methods,respectively.The coefficients of variation were less than 15%.The limits of detection(LOD)and the limits of quantification(LOQ)from lyophilization and QuEChERS method were 0.1 to 2.0μg/L and 0.2 to 5.0μg/L,respectively.