摘要
[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／mL，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＝27200X－0．00931，R＝1．0000；丙酸睾酮：Y＝13800X－0．000147，R＝1．0000；氯丙嗪：Y＝0．0951X＋0．0257，R＝0．9999；玉米赤霉醇：Y ＝44100X －0．00658，R ＝1．0000；己烯雌酚：Y ＝0．0934X ＋0．0188，R ＝0．9989。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。
Abstract
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.
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维普
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