建立了固相萃取-气相色谱-质谱法快速检测柑橘中55种农药多残留的分析方法。样品用乙腈均质提取,盐析除水液液萃取,石墨炭黑-氨基串联柱净化后用气相色谱-质谱仪(GC-MS)分析。采用选择离子监测模式(SIM),以保留时间和特征离子定性、峰面积定量。方法的检出限(S/N=3)为0.003 8～0.066 mg/kg,方法回收率为45.0%～137.5%,相对标准偏差<20%。

A method for the rapid determination of 55 pesticide residues in citrus by gas chromatography-mass spectrometry(GC-MS) with solid-phase extraction was proposed.The samples were extracted with acetonitrile,separated with liquid-liquid partitioning.The clear supernatant liquid purified by solid phase extraction was used for GCMS analysis.Determinations were performed by using selected ion monitoring(SIM) mode and external standard method was used in the quantification.Under the optimal conditions,the detection limits(S/N = 3) were in the range of 0.003 8 ～ 0.066 mg/kg.Tests for recovery were made by addition of mixed standards and the results were 45.0% ～ 137.5%,and the relative standard deviations were less than 20%.