高效液相色谱-串联质谱法测定动物源性食品中乙基多杀菌素残留

Determination of spinetoram residues in animal derived foods by high performance liquid chromatography-tandem mass spectrometry

目的建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)测定动物源性食品(牛奶、鸡肉、猪脂肪)中乙基多杀菌素残留量的分析方法。方法采用改进的QuEChERS法,样品经乙腈提取后,乙二胺-N-丙基硅烷化硅胶(primary second aryamine,PSA)、十八烷基硅烷键合硅胶(C_(18))和无水硫酸镁共同萃取净化,再经高效液相色谱-串联质谱法多反应监测(multiple reaction monitoring,MRM)模式扫描,基质匹配标准曲线外标法定量。结果乙基多杀菌素在0.001~1.000mg/L范围内线性关系良好,相关系数(r)均大于0.99。在3个添加水平下,平均回收率为73.8%~103.0%,相对标准偏差为1.7%~6.4%,牛奶、鸡肉和猪脂肪的定量限分别为0.010、0.001、0.050 mg/kg。结论该方法简单易行、回收率和重复性良好,可满足动物源性食品中乙基多杀菌素残留的实际监测。

Objective To establish a method for the determination of spinetoram residues in animal derived foods(milk,chicken and pig fat)by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods Using modified QuEChERS method,samples were extracted with acetonitrile,purified by primary secondary amine(PSA),C_(18)and magnesium sulfate anhydrous,then analyzed by HPLC-MS/MS in multiple reaction monitoring(MRM)mode,and quantified by matrix matching standard curve external standard method.Results Spinetoram had good linear relationships within the concentration ranges of 0.001-1.000 mg/L,and the correlation coefficients(r)were greater than 0.99.Under 3 kinds of spiked concentration levels,the average recoveries of spinetoram were 73.8%-103.0%,and the relative standard deviations were 1.7%-6.4%,the limits of quantitation of milk,chicken and pig fat were 0.010,0.001 and 0.050 mg/kg respectively.Conclusion This method is simple and easy to do,has good recovery and repeatability,and can meet the actual monitoring of spinetoram residues in animal derived foods.