固相萃取液相色谱串联质谱法测定生姜中涕灭威及其代谢产物

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

建立了固相萃取-液相色谱串联质谱法测定生姜基质中涕灭威及其代谢产物涕灭威亚砜、涕灭威砜的分析方法。试样经乙腈提取,氨基SPE小柱净化后,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:3种目标物在10ng/mL到50ng/mL质量浓度范围内呈现良好的线性,方法的检出限均为2μg/kg,3个加标水平下平均回收率在72～94%之间。该方法准确、灵敏、重现性好,可用于生姜样品中涕灭威及其代谢产物涕灭威亚砜、涕灭威砜的实际检测。

A comprehensive analytical method based on high performance liquid chromatography tandem mass spectrometry was developed for the determination of aldicarb,aldicarb sulfoxide,aldicarb sulfone residues in ginger. Samples were extracted with acetonitrile,and then the extract was purified with soild phase extraction（ SPE） 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 in the range of 10 ～50ng/mL and the limits of detection for the method were 2.0μg/kg. The mean recoveries at three spiked concentration levels were between 72% and 94%.The method is reliable,sensitive and reproducible,and could be rapidly applied in the determination of aldicarb,aldicarb sulfoxide,aldicarb sulfone residues in ginger.