采用超高效液相色谱-串联质谱法测定水产品中敌百虫、敌敌畏、甲胺磷的的含量。试样经0.1%甲酸-乙酸乙酯超声萃取，HC-C18固相萃取柱净化后，UPLC BEH C18色谱柱分离，选择离子监测（SIM），定量离子对（m/z）：258.7/127.0（敌百虫）、221.0/127.1（敌敌畏）、142.1/94.1（甲胺磷）；定性离子对（m/z）：258.7/109.0（敌百虫）、221.0/109.1（敌敌畏）、221.0/112.0（甲胺磷）。结果表明：敌百虫、敌敌畏、甲胺磷加标回收率在90.6%～106.0%之间，相对标准偏差不大于8.8%；以信噪比RSN=3计算，方法检出限均为1.5μg/kg，方法定量限均为5.0μg/kg。%A method for determining the residues of trichlorfon, dichlorvos and methamidophos in aquatic products was established by an ultra performance liquid chromatography tandem mass spectrometry. Samples was ultrasonic extracted with 0.1%formic acid-ethyl acetate, and purified with SPE-C18, and separated by UPLC BEH C18 column, and measured by selected ion monitoring (SIM). The qualitative ion pair (m/z) was 258.7/127.0(trichlorfon), 221.0/127.1(dichlorvos), and 142.1/94.1(methamidophos); the quantitative ion pair(m/z) was 258.7/109.0(trichlorfon), 221.0/109.1(dichlorvos), 221.0/112.0(methamidophos). The results showed that the recoveries were between 92.3%-106.0%, and the relative standard deviation were no more than 8.8%;According to RSN=3, the detection limits were 1.5μg/kg quantitative, limits were 5.0μg/kg.
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