粮食中磺酰脲类除草剂的UPLC/MS/MS测定方法  

Determination of sulfonylurea herbicides in grain by UPLC/MS/MS

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

机构地区：[1]天津市农业科学院中心实验室,天津300381

出　　处：《分析试验室》2012年第6期63-69,共7页Chinese Journal of Analysis Laboratory

基　　金：天津市农业科学院院长基金(09001)资助

摘　　要：建立了多类粮食作物中15种磺酰脲类除草剂的超高效液相色谱-串联质谱联用仪(UPLC/MS/MS)多离子监测(MRM)的多残留检测方法。样品经乙腈提取,乙腈饱和的正己烷液-液分配,石墨化碳氨基小柱净化,采用UPLC-MS/MS(ESI+)测定。方法中各种磺酰脲类除草剂在5～200μg/L浓度范围内线性良好,相关系数在0.9995～0.9999。在5～100μg/kg范围内,平均加标回收率在71.6%～115.3%之间,相对标准偏差不大于15%。各种药物的定量限(S/N≥10)均可达到5μg/kg。该方法可同时满足大豆、大米、玉米等多种粮食中磺酰脲类除草剂的检测需求。An ultra performance liquid chromatography-tandem mass spectrometric（UPLC/MS/MS） method was developed for the determination of the fifteen sulfony-lurea herbicides in grain.The samples were extracted with acetonitrile followed by liquid-liquid partition with hexane,cleaned-up by Carbon/NH2 solid phase and finally determined by UPLC/MS/MS in multiple reaction monitoring（MRM） mode with positive electrospray ionization（ESI＋）.All the standard calibration curves for fifteen sulfonylurea herbicides showed high correlation coefficients over the range of 2~200 μg/L,with the correlation coefficients between 0.9995 and 0.9999.The average recoveries of the fifteen sulfonylurea herbicides between 5 μg/kg and 100 μg/kg were between 71.6% and 115.3%,with the relative standard deviations（RSDs） less than 15%.The limits of quantification（S/N≥10） of all the fifteen sulfonylurea herbicides were 5 μg/kg.These indicated that the method developed in this study is easy,fast and sensitive,and it can meet the requirements of the multiple pesticide residue analysis.So,this method can be further applied to the detection of sulfonylurea herbicides in grain.

关 键 词：磺酰脲类除草剂 粮食 多残留 超高效液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学]