QuEChERS-气相色谱-串联质谱检测水牛乳中27种农药残留

Determination of 27 pesticide residues in buffalo milk by QuEChERS-gas chromatography-tandem mass spectrometry

基于QuEChERS前处理技术,建立通过气相色谱-串联质谱(GC-MS/MS)测定水牛乳中27种农药残留的方法。10 g水牛乳样品用10 mL乙腈溶液提取,经QuEChERS净化剂[900 mg无水硫酸镁、400 mg N-丙基乙二胺(PSA)、50 mg十八烷基硅烷(C_(18))、50 mg石墨化炭黑(GCB)]净化,采用GC-MS/MS测定。结果表明:炔丙菊酯在0.015~0.500μg/mL、另26种农药在0.005~0.500μg/mL范围内线性关系良好(r≥0.9994)。方法的检出限为0.01~8 ng/kg,定量限为0.03~27 ng/kg,平均回收率为76%~111%,相对标准偏差(RSD)为1.5%~5.9%。建立的样品前处理方法简易快速、节省试剂、净化效果佳。

A method for determining 27 pesticide residues in buffalo milk by gas chromatography-tandem mass spectrometry(GC-MS/MS)was established based on QuEChERS pre-treatment technique.Buffalo milk sample of 10 g was extracted with 10 mL acetonitrile solution,purified by QuEChERS(900 mg anhydrous MgSO_(4),400 mg PSA,50 mg C_(18),50mg GCB),and then detected by GC-MS/MS.The results showed that the linear relationship of prallethrin in the range of 0.015-0.500μg/mL and the other 26 pesticides in the range of 0.005-0.500μg/mL was good(r≥0.9994).The detection limits were 0.01-8 ng/kg,and the quantization limits were 0.03-27 ng/kg.The average recovery rate was 76%-111%,and the relative standard deviation(RSD)was 1.5%-5.9%.The method was simple,rapid and reagent-economical,with good purification effect.