高效液相色谱-串联质谱检测小麦中噻虫胺残留量

Analysis of Clothianidin Residue in Wheat by HPLC-MS/MS

建立了高效液相色谱-串联质谱法(HPLC-MS/MS)快速检测小麦及其秸秆中噻虫胺残留。样品经乙腈提取,C_(18)吸附剂净化,多反应监测模式检测,基质匹配标准品外标法定量。当质量浓度为0.01～1 mg/L时,噻虫胺在基质中的质量浓度与峰面积呈良好的线性关系,相关系数为0.999 3～0.999 9。在0.02～1 mg/kg添加水平下,噻虫胺在小麦、最终秸秆和青秸秆中的平均回收率为87%～105%,相对标准偏差为2%～18%。噻虫胺在小麦中的定量限为0.02 mg/kg。该方法简便、快速、准确,可用于小麦中噻虫胺的残留检测。

A method for the determination of clothianidin residues in wheat and straw was established by HPLC-MS/MS.The samples were extracted with acetonitrile and purified with C18.The clothianidin residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect.The results indicated that the calibration curves of clothianidin were linear in the range of 0.01-1 mg/L with the correlation coefficients of 0.999 3-0.999 9.When the addition level ranged from 0.02 to 1 mg/kg,the average recoveries of clothianidin in wheat,straw and green straw were 87%-105%,and the relative standard deviations were 2%-18%.The limits of quantitation(LOQ)were all 0.02 mg/kg.This method was simple,rapid and accurate,and could be adapted for the confirmation of clothianidin residues in wheat samples.