QuEChERS-气相色谱-三重四级杆串联质谱法高通量检测生鲜肉中有机磷农药残留  

High-throughput detection of organophosphorus pesticide residues in fresh meat by QuEChERS-GC-MS/MS

作　　者：王莎莎 沈习习 李曼曼 沈娟[1,2,3] 唐长波 王玮 WANG Shasha;SHEN Xixi;LI Manman;SHEN Juan;TANG Changbo;WANG Wei(College of Food Science and Technology,Nanjing Agricultural University,Nanjing 210095,China;National Center of Meat Quality and Safety Control,Nanjing Agricultural University,Nanjing 210095,China;Supervision,Inspection and Testing Center for Quality of Meat-products(Nanjing),Ministryof Agriculture and Rural Affairs,Nanjing Agricultural University,Nanjing 210095,China)

机构地区：[1]南京农业大学食品科技学院,江苏南京210095 [2]国家肉品质量安全控制工程技术研究中心(南京农业大学),江苏南京210095 [3]农业农村部肉及肉制品质量监督检验测试中心(南京)(南京农业大学),江苏南京210095

出　　处：《食品与发酵工业》2022年第5期262-265,I0004-I0007,266,267,共10页Food and Fermentation Industries

基　　金：国家重点研发计划政府间国际科技创新合作重点专项(2019YFE0103800)。

摘　　要：该研究旨在建立一种快速、有效检测生鲜肉中18种有机磷农药(organophosphorus pesticides, OPPs)残留的QuEChERS-GC-MS/MS检测方法。样品经饱和正己烷的乙腈溶液提取,MgSO;、CH;COONa、N-丙基乙二胺(N-propyl ethylenediamine, PSA)、十八烷基键合硅胶(C_(18))分散固相萃取净化后,采用DB-1701色谱柱进行分离,GC-MS/MS检测。有机磷农药在1~100μg/kg线性关系良好,相关系数(R^(2))均>0.990 0,检出限为0.02~0.74μg/kg,定量限为0.08~2.48μg/kg,加标回收率为76%~106%,相对标准偏差为0.50%~7.9%。该实验建立的QuEChERS-GC-MS/MS方法可同时检测18种有机磷农药,操作简便、快速、灵敏、准确,能够满足生鲜畜禽肉中有机磷农药残留的高通量快速检测。This study aimed to establish a rapid and effective QuEChERS-GC-MS/MS detection method for 18 organophosphorus pesticide residues in fresh meat. The sample was extracted with saturated n-hexane in acetonitrile and purified by dispersion solid-phase extraction with MgSO;, CH;COONa, N-propyl ethylenediamine(PSA) and octadecyl bonded silica gel(C_(18)). Then DB-1701 capillary column was used for the separation, and GC-MS/MS was used for the detection. Organophosphorus pesticides showed a good linear relationship in the range of 1-100 μg/kg, and the square of correlation coefficient(R^(2)) were all greater than 0.990 0. The detection limit was 0.02-0.74 μg/kg and the quantification limit was 0.08-2.48 μg/kg. Meanwhile, the recovery rate reached 76%-106% and the relative standard deviation was 0.50%-7.9%. The QuEChERS-GC-MS/MS method established in this study can simultaneously detect 18 organophosphorus pesticides. It is simple, fast, sensitive and accurate, which can meet the high throughput and rapidity of organophosphorus pesticide residues in fresh livestock and poultry meat.

关 键 词：有机磷农药 生鲜肉 QUECHERS 气相色谱-三重四级杆质谱 检测 

分 类 号：O657.63[理学—分析化学] TS251.7[理学—化学]