UPLC-MS/MS测定土壤中的甲磺隆、苄嘧磺隆残留

建立了超高效液相色谱串联质谱法检测土壤中甲磺隆、苄嘧磺隆残留的方法。土壤中的甲磺隆和苄嘧磺隆经C18固相萃取小柱萃取,然后用Waters Acquity UPLC BEH C18色谱柱（50mm×2.1mm,1.7μm）分离,以0.05%乙酸-甲醇为流动相进行梯度洗脱,流速0.4mL.min-1,采用正离子电喷雾电离模式测定,外标法定量。本方法简便、快速、准确、可靠,甲磺隆、苄嘧磺隆在1.0—100.0μg.L-1的浓度范围内呈良好的线性关系,相关系数（r）分别为0.9997和0.9999;检出限分别为0.02μg.kg-1和0.03μg.kg-1,回收率为86.2%—96.5%,相对标准偏差不大于5.1%。

Determination of Residues of Metsulfuron-Methyl and Bensulfuron-Methyl in Soil by UPLC-MS/MS

The method for the determination of the residues of metsulfuron-methyl and bensulfuron-methyl in soil was established by ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS）.The residues of metsulfuron-methyl and bensulfuron-methyl were extracted with solid phase extraction C18,and the separation of metsulfuron-methyl and bensulfuron-methyl were performed on Waters Acquity UPLC system with a BEH C18 column（50mm×2.1mm,1.7μm） with a linear gradient elution（methyl alcohol：0.05% acetic acid as mobile phase） at a flow rate of 0.4mL·min-1,and that were detected by MS/MS with positive electrospray ionization mode.The methods were quantified by external standard method.The calibration curves were good linear between the concentrations of 1.0—100.0μg·L-1,and correlation coefficients（r） were 0.9997 and 0.9999 for metsulfuron-methyl and bensulfuron-methyl,respectively.The detection limits for metsulfuron-methyl and bensulfuron-methyl were 0.02μg·kg-1 and 0.03μg·kg-1,respectively,and the recoveries were in the range of 86.2%—96.5% with the RSD not more than 5.1%.This method is proved to be simple,fast,reliable and accurate.