凝胶渗透色谱净化联合气相色谱-串联质谱法同时测定番石榴中3种农药残留

目的建立一种同时测定番石榴中3种常用农药的凝胶渗透色谱净化联合气相色谱-串联质谱法(gel permeation chromatography-gas chromatography-tandem mass spectrometry,GPC-GC-MS/MS)分析方法。方法番石榴样品经乙腈提取,凝胶渗透色谱净化,毛细管气相色谱柱分离后,采用三重串联四极杆多反应监测模式测定。结果 3种农药在0.05~0.50 mg/L范围内线性关系良好,相关系数均不低于0.9990;毒死蜱、克螨特、氟氯氰菊酯的定量限分别为0.002、0.005、0.01 mg/kg;在0.05、0.10、0.50 mg/kg 3个加标水平下,3种农药的回收率在83.3%~104.8%之间,相对标准差为2.9%~7.9%。结论该方法处理简便,能满足番石榴中3种常用农药毒死蜱、克螨特、氟氯氰菊酯残留检测的要求。

Simultaneous determination of 3 kinds of pesticide residues in guava by gel permeation chromatography-gas chromatography-tandem mass spectrometry

Objective To develop an analysis method for determination of 3 kinds of pesticide residues in guava by gel permeation chromatography-gas chromatography-tandem mass spectrometry (GPC-GC-MS/MS). Methods The guava samples were extracted by acetonitrile, followed by a cleanup procedure with GPC, and then separated by capillary gas chromatography column. Finally, the concentrated solution was analyzed by triple tandem quadrupole multiple reaction monitoring (MRM). Results The correlation coefficients (r2) of 3 kinds of tested pesticides were greater than 0.9990 within their respective linear ranges of 0.05~0.50 mg/L. The limits of quantitation (LOQ) for chlorpyrifos, propargite and cyfluthrin were 0.002, 0.005 and 0.01 mg/kg, respectively. The average recoveries of three pesticides were 83.3%~104.8% when the spiked levels were 0.05, 0.10 and 0.50 mg/kg, with relative standard deviations (RSDs) in the range of 2.9%~7.9%. Conclusions The method is easy, and can satisfy for detection of chlorpyrifos, propargite and cyfluthrin residues in guava.