固相萃取/高效液相色谱-串联质谱法测定食品中涕灭威及其代谢产物涕灭威亚砜与涕灭威砜残留量

Determination of Aldicarb,Aldicarb Sulfoxide,Aldicarb Sulfone Residues in Foods by Solid Phase Extraction/High Performance Liquid Chromatography Tandem Mass Spectrometry

建立了高效液相色谱-串联质谱法测定生姜、番茄、菠菜、大米、杏仁、花生、大豆、苹果、柑橘、茶叶、猪肝、鸡肉12种基质中涕灭威、涕灭威砜、涕灭威亚砜残留量的分析方法。试样经乙腈提取,氨基SPE小柱净化后,以Agilent色谱柱(3.5μm,100 mm×2.1 mm)分离,采用多反应监测(MRM)正离子模式检测,外标法定量。实验结果表明:涕灭威、涕灭威砜、涕灭威亚砜在0.01～0.2 mg/L质量浓度范围内呈良好线性。方法的检出限为0.002 mg/kg,定量下限为0.01 mg/kg。在低、中、高3个加标水平下的平均回收率为68%～89%。该方法准确、灵敏、重现性好,可用于不同样品中涕灭威、涕灭威砜、涕灭威亚砜残留量的实际检测。

A comprehensive analytical method based on high performance liquid chromatography tandem mass spectrometry（HPLC -MS/MS） was developed for the determination of aldicarb, aldicarb sulfone and aldicarb sulfoxide residues in ginger, tomato, spinach, rice, peanut, soybeans, almonds, apples, citrus, tea, liver and chicken samples. Various samples were extracted with acetonitrile. The extract was purified with soild phase extraction （SPE） column, and then separated on an Agilent（3.5 μm, 100 mm ×2. 1 mm） column. The detection was performed by MS/MS under positive electrospray ionization and multiple reaction monitoring（MRM） mode, with the external standard method. The result indicated that the calibration curves showed good linearities for aldicarb, aldicarb sulfone and ablicarb sulfoxide in the range of 0.01 -0. 2 mg/L. The limit of detection for the method was 0. 002 mg/kg and the limit of quantitation was 0.01 mg/kg. The mean recoveries at three spiked concentration levels （low, middle, high ） were between 68% and 89% . The method is reliable, sensitive and reproducible, and could be rapidly applied in the determination of aldicarb, aldicarb sulfone and aldicarh sulfoxide residues in different foods.