超高效液相色谱-串联质谱法测定鸡肉中硝基呋喃类药物残留

Determination of nitrofurans residues in chicken by UPLC-MS /MS

目的建立超高效液相色谱-串联质谱法测定鸡肉中硝基呋喃类药物代谢物残留的方法。方法采用对样品衍生化处理,Oasis HLB固相萃取小柱净化后,超高效液相色谱-串联质谱测定。色谱柱:AQUITY UPLC BEH C18(2.1 mm×100 mm,1.7μm);柱温:40℃;样品室温度:4℃;流动相:A相为甲醇,B相为0.1%甲酸水,梯度洗脱;流速:0.3 ml/min;进样体积:10μl;多反应监测(MRM)模式检测。结果最低检出限呋喃它酮代谢物、呋喃唑酮代谢物为0.005μg/kg,呋喃妥因代谢物、呋喃西林代谢物为0.01μg/kg。呋喃它酮代谢物、呋喃唑酮代谢物、呋喃妥因代谢物、呋喃西林代谢物的平均回收率和RSD分别为95%(RSD=2.7%)、95%(RSD=1.9%)、93%(RSD=2.1%)、92%(RSD=1.5%)。结论本方法检出限低,精密度高,适用于鸡肉中硝基呋喃类药物代谢物的检测。

Objective To establish an ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS /MS） method for determination of nitrofurans metabolite residues in chicken.Methods The chicken samples were derivatized and purified with Oasis HLB SPE column,then determined by UPLC-MS /MS under multiple reaction monitoring mode.The chromatographic column was AQUITY UPLC BEH C18（2.1 mm ×100 mm,1.7 μm）,with column temperatue at 40 ℃,sample temperatue at 4 ℃.Methanol as A mobile phase and 0.1% formic acid water as B mobile phase were used for gradient elution.The flow rate was 0.3 ml /min and the injection volume was 10 μl.Results The detection limits of AMOZ and AOZ were both 0.005 μg /kg,while those of AHD and SEM were both 0.01 μg /kg.The recoveries of AMOZ,AOZ,AHD and SEM were95%,95%,93% and 92% respectively,and the RSDs were 2.7%,1.9%,2.1%,1.5%.Conclusion The method has low detection limit and high precision,and it is suitable for determination of nitrofuran metabolites in chicken.