UHPLC-MS/MS法测定大米中丁草胺和吡虫啉残留

Determination of Butachlor and Imidacloprid Residue in Rice by UHPLC-MS/MS

为建立大米中丁草胺和吡虫啉残留农药残留的检测方法,采用超高效液相色谱-串联质谱的方法,样品经乙腈提取,弗罗里硅土固相萃取柱净化,采用多反应监测模式(MRM),对流动相比例、柱温、流速、碎裂电压、碰撞能等条件进行了优化。结果表明:丁草胺和吡虫啉在1~250μg·kg-1范围内保持良好线性关系且(r>0.999 5)回收率在88.7%~105.4%,检出限分别为0.27μg·kg-1和0.43μg·kg-1,定量限为0.89μg·kg-1和1.42μg·kg-1,RSD小于3.9%。该方法稳定、可靠,可满足大米中丁草胺和吡虫啉农药残留检测的需要。

UHPLC-MS/MS method was developed for determination of butachlor and imidacloprid residues in rice. After extracted with aeetonitrile,riee samples were cleaned up by florisil solid-phase extraction column purification. The mass spectrometer was op- erated in the positive mode using MRM. Influences of mobile phases, column temperature,flow velocity,fragmentor,collison energy were investigated.The method maintained good linear range（r〉0.999 5 ）with recovery 88.7%-105.4%, and the limits of detection were 0.27μg·kg^-1 and 0.43μg·kg^-1,the limits of quantification were 0.89 μg·kg^-1 and 1.42 μg·kg^-1,when the concentration of Butachlor and imidacloprid was 1 ~250 μg·kg^-1. The method was efficient,reliable and could meet the requirements for the determination of butachlor and imidacloprid residue.