小麦中多种磺酰脲类除草剂的UPLC-MS/MS分析方法研究  

Simultaneous Determination of Eleven Sulfonylurea Herbicides in Wheat by UPLC-MS/MS

作　　者：李辉[1] 李娜[1] 张玉婷[1] 郭永泽[1] 邵辉[1] 刘磊[1] 宋淑荣[1] 

机构地区：[1]天津市农业科学院中心实验室,天津300381

出　　处：《安徽农业科学》2012年第12期7143-7144,7282,共3页Journal of Anhui Agricultural Sciences

基　　金：天津市农业科学院院长基金(09001)

摘　　要：[目的]用超高效液相色谱-串联四极杆质谱(UPLC-MS/MS),在多反应监测(MRM)模式下,建立小麦中11种磺酰脲类除草剂残留的定性定量分析方法。[方法]样品经乙腈提取,乙腈饱和的正己烷液-液分配,用弗罗里硅土小柱净化,采用UPLC-MS/MS(ESI+)测定。[结果]在2～200μg/L浓度范围内方法中各种磺酰脲类除草剂线性良好,相关系数在0.999 8和0.999 9之间。在5,25和50μg/kg 3个添加浓度水平下的平均回收率在76.2%和102.4%之间,相对标准偏差不大于10%。[结论]该方法快速简便,可满足小麦中多种磺酰脲类除草剂的检测要求。[Objective] To develop a quantitative analysis method for eleven sulfonylurea herbicides in wheat by an ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS） method in the multiple reaction monitoring（MRM） mode.[Method] The samples were extracted with acetonitrile,followed by liquid-liquid partition with hexane,after being cleaned-up by an magnesiumsilicate solid phase,the sample was analyzed by UPLC-MS/MS in multiple reaction monitoring（MRM） mode.[Result] The sulfonylurea herbicides showed good linear relations within the concentration range of 2-200 μg/L,with the correlation coefficients between 0.999 8 and 0.999 9.The average recoveries of the eleven sulfonylurea herbicides at the three levels of 5,25 and 50 μg/kg were between 76.2% and 102.4%,with the relative standard deviation（RSD） less than 10%.[Conclusion] This method is rapid and simple and can be further applied to detection of sulfonylurea herbicides in wheat.

关 键 词：磺酰脲类除草剂 小麦 多残留 超高效液相色谱-串联质谱 

分 类 号：S512.1[农业科学—作物学]