气相色谱-串联质谱法结合QuEChERS方法快速检测柑橘中52种农药多残留.pdf

152 2013, Vol.34, No.06 食品科学 ※分析检测 气相色谱-串联质谱法结合QuEChERS方法 快速检测柑橘中52种农药多残留 1 2 1,2,3,* 张雪莲 ，张耀海，焦必宁 (1.西南大学食品科学学院，重庆 400715 ；2.农业部柑橘产品质量安全风险评估实验室(重庆)， 中国农业科学院柑桔研究所，重庆 400712 ；3. 国家柑桔工程技术研究中心，重庆 400712) 摘  要：建立气相色谱- 串联质谱结合QuEChERS方法快速检测柑橘中52种农药多残留。样品经乙腈提取、无水 N 硫酸镁和氯化钠盐析后，用 -丙基乙二胺(PSA) 固相材料分散填料净化，用气相色谱- 串联质谱在多反应监测模式 (MRM)下分析检测，该方法的检出限(R SN=3)为0.07～5.7μg/kg ，平均回收率为77.3%～117.8%，相对标准偏差小于 13.8%。该方法简单、快速、安全、便宜、重现性好，适用于柑橘类水果农药多残留检测。 关键词：柑橘；农药残留；QuEChERS ；气相色谱- 串联质谱法 Rapid Determination of 52 Pesticide Residues in Citrus by Gas Chromatography-Tandem Mass Spectrometry Coupled with QuEChER 1 2 1,2,3,* ZHANG Xue-lian ，ZHANG Yao-hai ，JIAO Bi-ning (1. College of Food Science, Southwest University, Chongqing 400715, China；2. Laboratory of Quality Safety Risk Assessment for Citrus Products (Chongqing), Ministry of Agriculture, Citrus Research Institute, Chinese Academy of Agricultural Sciences, Chongqing 400712, China ；3. National Citrus Engineering Research Center, Chongqing 400712, China) Abstract ：In this study, an analytical method was established for the determination of 52 pesticide residues in citrus fruits using QuEChERS cleanup and gas chromatography-tandem mass spectrometry (GC-MS/MS). The pesticide residues in citrus fruit samples were extracted into acetonitrile and salted out by anhydrous MgSO4 and NaCl. Then, the pesticide residues in the supernatant after clean-up on the sorbents of N-propyl ethylene diamine (PSA) were subjected to GC-MS/MS analysis under multi-reaction monitoring (MRM) mode. The limit of detect