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

中文关键词:  动物源性食品  乙基多杀菌素  高效液相色谱-串联质谱法

英文关键词:animal derived foods  spinetoram  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      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 secondary amine, PSA)、十八烷基硅烷键合硅胶(C18)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0.001~1.000 mg/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。

英文摘要:

      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), C18 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.