氧化石墨烯分散固相萃取-LC-MS/MS法检测花生油中涕灭威及其代谢物残留

Determination of aldicarb and its metabolites residues in peanut oil by graphene oxide DSPE combined with LC-MS/MS

建立了氧化石墨烯分散固相萃取—液相色谱串联质谱法(LC-MS/MS)检测花生油中涕灭威及其代谢物涕灭威砜和涕灭威亚砜3种农药残留的方法。样品经乙腈提取,以氧化石墨烯分散固相萃取净化后,注入LC-MS/MS检测。色谱柱采用Poroshell 120 EC-C18(3.0×100 mm,2.7μm),在多反应监测模式下检测,外标法定量。结果表明:上述3种农药在浓度5~150μg/L范围内线性关系良好,相关系数r=0.991~0.999,方法检测限为0.6~1.8μg/kg,在不同添加水平下,平均回收率为62%~103%。该方法简便、快速、成本低,能够满足花生油中涕灭威及其代谢物的检测要求。

A method was established to determine three pesticides residues,aldicard and its metabolites aldicarb-sulfone and aldicarb-sulfoxide,in peanut oil by graphene oxide dispersive solid phase extraction（DSPE） combined with liquid chromatography-tandem mass spectrum（LC-MS/MS）.The sample was extracted by acetonitrile and purified by graphene oxide with DSPE and then separated by LC with Poroshell 120 EC-C18,3.0×100 mm,2.7 μm column.The analysis was carried out in the multi-reaction monitoring mode and external standard method was used for quantification.The results showed that the calibration curve of the three pesticides showed a good linear relationship in the range of 5~150μg/L with the correlation coefficient r = 0.991~0.999,the detection limit of the method was 0.6~1.8μg/kg,and the average recovery was 62%~103%at different level.The method is simple,fast,cheap,can meet the requirements of the determination of aldicard and its metabolites residues in peanut oil.