高效液相色谱串联质谱法测定烟草中有机磷农药残留量

Determination of Organophosphorous Pesticide Residues in Tobacco with LC-MS/MS

用水和乙腈混合液（体积比1：1）提取，提取液经无水硫酸镁和PSA吸附剂处理，及0．45μm滤膜过滤后，以甲醇／水溶液作流动相，流速1mL／min，采用高效液相色谱-串联质谱法于多反应监测（MRM）模式下同时测定了烟草中15种有机磷农药的残留量。检测限为2．58～11．5μg／kg，回收率66％～104％，相对标准偏差不大于8．99％．

A method based on liquid chromatography tandem mass spectrometry （LC-MS/MS） was developed for simultaneously determining the residues of 15 organophosphorus pesticides in tobacco. The samples were extracted with 50% （v/v） acetonitrile water solution, the extracts were cleaned up with primary secondary amine （PSA） adsorbent and magnesium sulfate, then filtrated by 0.45 μm filter membrane, and analyzed by LC-MS/MS with multiple reaction monitoring （MRM） mode, using water containing 0.05% acetic acid and methanol as a mobile phase at the flow rate of 1 mL/minute. The limits of detection and the recoveries of the organophosphorous pesticides were 2.58 to l 1.5 μg/kg and 66% to 104% , respectively, with RSDs of below 8.99%.