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

Rapid Determination of 52 Pesticide Residues in Citrus by Gas Chromatography-Tandem Mass Spectrometry Coupled with QuEChER

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、无水硫酸镁和氯化钠盐析后,用N-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(RSN=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。

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 NaC1. 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 detection （RsN = 3） of the established method were in the range of 0.07-5.7 μg/kg, and the average recovery rates for 52 pesticide residues in a blank sample were 77.3%-117.8% with a relative standard deviation （RSD） less than 13.8%. Therefore, this method is simple, quick, safe, cheap and reproducible so that it is suitable for the detection of multiple pesticide residues in citrus fruit samples.