水产品中辛硫磷、倍硫磷和蝇毒磷的超高效液相色谱-串联质谱法检测

Detection of phoxim,fenthion and coumaphos in aquatic products by UPLC-MS/MS

[目的]建立了水产品中辛硫磷、倍硫磷和蝇毒磷3种有机磷农药的检测方法。[方法]样品经酸化乙腈提取,PSA吸附剂分散固相萃取净化,超高效液相色谱-串联质谱在多反应离子监测模式下检测,基质匹配外标法定量。结果加标浓度在10~100μg/kg范围内,线性相关系数(R)大于0.99。3种有机磷农药的平均回收率范围为65.8%~101.0%,RSD范围为11.4%~16.0%。本方法检出限为10μg/kg,定量限为20μg/kg。[结论]该方法可用于水产品中辛硫磷、倍硫磷和蝇毒磷等3种有机磷农药残留的同时测定。

[ Aim ] A method was developed for determining simultaneously of phoxim, fenthion and coumaphos resi- dues in aquatic products. [ Method ] The samples were extracted with acidic acetonitrile, cleaned up using PSA adsorbent, detected quantitatively by UPLC-MS/MS with external standard method by matrix-match standard solution. [ Result ] At the spiked level of 10 -100 μg/kg, the linear correlation coefficient （R） is greater than 0.99, the average recoveries of the 3 organophosphorus pesticides were ranged from 65.8% to 101.0% with 11.4% - 16.0% relative standard deviations . The detection limit of these three pesticides was 10 μg/kg and the quantitation limit was 20 p.g/kg. [ Conclusion ] The method was simple and reliable, and could meet the requirement of 3 organophosphorus pesticide residue analysis. It could be applied to determine simultaneously phoxim, fenthion and coumaphos in aquatic products.