气液微萃取仪联用气相色谱-质谱仪检测果蔬中农药残留量

Detection of pesticide residues in fruits and vegetables by gas-liquid microextraction combined with gas chromatography-mass spectrography

目的建立气液微萃取仪(gas-liquid microextraction,GLME)与气相色谱质谱联用仪(gas chromatographymass spectrography,GC-MS)测定食品中农药残留。方法称取0.1 g匀浆样品直接加入GLME中进行萃取净化,定容至100μL,结合内标法通过GC-MS检测分析。结果 30种农药在0.001~1 mg/kg浓度范围内线性良好,相关系数在0.9951~0.9999,检出限为0.001~0.021 mg/kg,定量限为0.003~0.070 mg/kg,平均回收率为67%~119%(n=3),相对标准偏差在1%~26%之间。结论该方法快速、准确,能满足果蔬类中多种农药残留的定性定量分析。

Objective To establish a method for the determination of pesticide residues in fruits and vegetables by gas-liquid microextraction（GLME） and gas chromatography-mass spectrometry（GC-MS）. Method The 0.1 g of homogeneous sample was directly added into GLME for extraction and purification. The volume was adjusted to 100 μL and the samples were analyzed by GC-MS with internal standard method. Result The 30 kinds of pesticide had good linear relationships in the range of 0.001-1 mg/kg, and the correlation coefficients were 0.9951-0.9999. The limits of detection were 0.001-0.021 mg/kg and the limits of quantitation were 0.003-0.070 mg/kg. The average recoveries were 67%-119%（n=3） with relative standard deviations of 1%-26%. Conclusion The method is fast and accurate, which can satisfy the quantitative analysis of various pesticide residues in fruits and vegetables.