HPLC-MS法测定猪肉中地西泮等5种禁用药物的残留量

目的]建立快速、准确、高灵敏度的测定猪肉中地西泮等5种禁用药物残留量的分析方法。方法]采用高效液相色谱-串联质谱联用法(HPLC-MS),通过不同的离子模式进行猪肉中5种禁用药物残留量的测定,其中地西泮、丙酸睾酮、氯丙嗪采用正离子模式,玉米赤霉醇以及己烯雌酚采用负离子模式,并进行多反应检测(MRM)。结果]试验显示,该方法的线性范围为:3~100 ng/m L,标准曲线线性良好,其回归方程及相关系数分别为地西泮:Y=27 200X-0.009 31,R=1.000 0;丙酸睾酮:Y=13 800X-0.000 147,R=1.000 0;氯丙嗪:Y=0.095 1X+0.025 7,R=0.999 9;玉米赤霉醇:Y=44 100X-0.006 58,R=1.000 0;己烯雌酚:Y=0.093 4X+0.018 8,R=0.998 9。回收率分别为:地西泮100.50%~111.30%;丙酸睾酮73.30%~84.20%;氯丙嗪70.30%~99.10%;玉米赤霉醇69.90%~75.30%;己烯雌酚84.70%~117.70%。最低检出限分别为:地西泮0.4μg/kg,丙酸睾酮0.6μg/kg,氯丙嗪0.3μg/kg,玉米赤霉醇0.5μg/kg,己烯雌酚0.8μg/kg。结论]该方法操作简便、快速,是动物源性食品中地西泮等5种禁用药物残留的快速而准确的检测方法。

Determination of Diazepam and Other Four Kinds of Banned Drugs in Pork by HPLC-MS

Objective] To establish a rapid, accurate, highly sensitive determination method for diazepam and other four kinds of banned drugs in the pork.Method] High performance liquid chromatography-tandem mass spectrometry (HPLC-MS) was used with different ion modes.Re-sidual quantities of five banned drugs in pork were detected.Among them, positive ion mode was used for diazepam, testosterone propionate and chlorpromazine;while negative ion mode was used for zearalanol and diethylstilbestrol . Result ] The linear range of this method was 3 -100 ng/mL; the standard curve had good linearity.Their regression equations and R values were as follows:diazepam:Y=27 200X-0.009 31 and R=1.000 0, respectively.Testosterone propionate:Y=13 800X-0.000 147, R=1.000 0;chlorpromazine:Y=0.095 1X+0.025 7, R=0.999 9; zearalanol: Y=441 00X-0.006 58, R=1.000 0; diethylstilbestrol: Y=0.093 4X+0.018 8, R=0.998 9.Recovery rates were:100.50%-111.30% for diazepam, 73.30%-84.20%for testosterone propionate, 70.30%-99.10%for chlorpromazine.69.90%-75.30%for zearalanol, 84.70%-117.70% for diethylstilbestrol.The minimum detection limits were:0.4μg/kg for diazepam, 0.6μg/kg for testoster-one propionate, 0.3 μg/kg for chlorpromazine, 0.5 μg/kg for zearalanol, and 0.8 μg/kg for diethylstilbestrol.Conclusion] This method is rapid, simple, sensitive and accurate, and it is a suitable method for rapid determination of diazepam and other four kinds of banned drugs in the animal derived food.