气相色谱-质谱联用快速检测柑橘中55种农药多残留

Rapid Determination of 55 Pesticide Residues in Citrus by Gas Chromatography with Mass Spectrometry Detection

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 GC- MS 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%.