超高效液相色谱-质谱串联法测定双孢菇中噻虫嗪及其代谢物噻虫胺残留量

Determination of Thiamethoxam and Its Metabolite Clothianidin Residues in Agaricus bisporus by UPLC-MS/MS

建立改进的QuEChERS提取净化方法和超高效液相色谱-串联质谱法测定双孢菇中噻虫嗪及其代谢物噻虫胺残留。样品经乙腈提取后,采用MgSO_4、PSA和C_(18)吸附净化,UPLC-MS/MS检测。研究结果表明,噻虫嗪和噻虫胺质量浓度为0.005～0.5 mg/L,方法呈良好的线性关系,相关系数大于0.995。方法的检出限为0.1 ng,定量限为0.005 mg/kg。在添加质量分数为0.005、0.01、0.5mg/kg时,方法的平均回收率为85%～112%,相对标准偏差为0.5%～7.1%。该方法准确可靠,灵敏度和准确度均达到了农药残留检测的要求。

A sensitive LC-MS/MS method for determining of thiamethoxam and its metabolite clothianidin residues in Agaricus bisporus was established by improved QuEChERS. The thiamethoxam and clothianidin residues in Agaricus bisporus were extracted by acetonitrile, purified by the mixture of MgSO4, PSA, C18, then determined by UPLC-MS/MS. The results showed that the good linearities of thiamethoxam and clothianidin were obtained at the concentration of 0.005-0.5mg/L, with the correlative coefficient more than 0.995. The detection limits of thiamethoxam and clothianidin in Agaricus bisporus were 0.1 ng, the quantification limits were 0.005mg/kg. When the spiked concentration of 0.005-0.5mg/L, the average recoveries of thiamethoxam and clothianidin were 85%-112%, and the variation coefficients were 0.5%-7.1%. The UPLC-MS/MS method was simple, the sensitivity and accuracy met the requirements of residue analysis.