QuEChERS结合气相色谱-串联三重四极杆质谱快速测定水产品中100种农药残留

Rapid Determination of Multiple Pesticide Residues in Aquatic Products by QuEChERS and Gas Chromatography-Tandem Mass Spectrometry

目的:建立QuEChERS结合气相色谱-串联三重四极杆质谱快速测定水产品中100种农药残留的方法。方法:样品经改进QuEChERS方法提取,分散固相萃取净化,通过气相色谱-串联三重四极杆质谱联用技术检测。结果:100种农药在0.005~0.500 mg/L范围内具有良好的线性关系,相关系数均大于0.995,对于5.00 g样品的100种农药的检出限范围为1.00×10^(–6)~2.97×10^(–3)mg/kg,定量限范围为2.00×10^(–6)~9.90×10^(–3)mg/kg,3个浓度添加水平的回收率在60.2%~120.0%,相对标准偏差(RSD,n=6)在0.26%~10.96%。结论:该方法具有操作简便、快速、可靠性强的特点,适用于鲩鱼、牛蛙、基围虾等水产品中多种农药残留的检测。

Objective:To establish a method for the rapid determination of 100 pesticide residues simuletaneously in aquatic products by gas chromatography-tandem mass spectrometry(GC-MS/MS)with QuEChERS.Methods:The samples were extracted by modified QuEChERS method,purified by dispersed solid phase extraction,and then the supernatant analyzed by GC-MS/MS.Results:The linear relationship was good within the range of 0.005–0.500 mg/L for 100 pesticide residues,with correlation coefficients higher than 0.995.The detection limit and quantitation limit were 1.00×10^(–6)–2.97×10^(–3)mg/kg and 2.00×10^(–6)–9.90×10^(–3)mg/kg,respectively.Overall recoveries and relative standard deviations(RSDs,n=6)were ranged from 60.2%to 120.0%and from 0.26%to 10.96%,respectively.Conclusion:The method has the advantages of simple operation,rapid and better reliability,which is suitable for the detection of a variety of pesticide residues in grass carp,bullfrog,prawn and other aquatic products.