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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。
Objective To establish a gel permeation chromatography-gas chromatography-tandem mass spectrometry (GPC-GC-MS / MS) method for the simultaneous determination of three commonly used pesticides in guava. Methods Guava samples were extracted with acetonitrile and purified by gel permeation chromatography (GC-MS). After separation by capillary gas chromatography (GC), the triple quadrupole reaction monitoring was used. Results The linearity of the three pesticides in the range of 0.05-0.50 mg / L was good, and the correlation coefficients were not lower than 0.9990. The limits of quantification of chlorpyrifos, propargite and cyfluthrin were 0.002,0.005 and 0.01 mg / kg, respectively. At 0.05, Under the three spiked levels of 0.10, 0.50 mg / kg, the recoveries of three pesticides ranged from 83.3% to 104.8% with relative standard deviations of 2.9% -7.9%. Conclusion The method is simple and easy to handle and can meet the requirements of the detection of chlorpyrifos, propargite and cyfluthrin residues in guava.