超高效液相色谱-串联质谱法测定稻田水体中的甲磺隆、苄嘧磺隆残留

建立了水体中甲磺隆、苄嘧磺隆残留检测的超高效液相色谱 串联质谱法。水样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（50 mm×2.1 mm×1.7 μm）分离，以0.05％乙酸/甲醇为流动相进行梯度洗脱，流速0.4 mL/min, 采用正离子电喷雾电离模式测定,外标法定量。结果表明：甲磺隆、苄嘧磺隆在1.0~500.0 μg/L的浓度范围内呈良好的线性关系，相关系数分别为0.999 7和0.999 9，检出限分别为0.002 5 μg/L和0.005 μg/L，回收率为87.6％~98.2％，相对标准偏差小于3.5％。

Determination of Metsulfuron-Methyl and Bensulfuron-Methyl in Paddyfield Water by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

Metsulfuron-methyl and bensulfuron-methyl in paddyfield water were determined by ultra performance liquid chromatography-tandem mass spectrometry（UPLC MS/MS）. The remains of metsulfuron-methyl and bensulfuron methyl were extracted with solid phase extraction C₁₈ cartridge.The separation of metsulfuron-methyl and bensulfuron-methyl was performed on Waters Acquity UPLC system with a BEH C₁₈ column (50 mm×2.1 mm×1.7 μm) and with a linear gradient elution (CH₃OH and 0.05% acetic acid as mobile phase) at a flow rate of 0.4 mL/min， and detected by MS/MS with positive electrospray ionization mode. The method used external standard for quantification. The calibration curves have good linear correlation in the concentration range of 1.0—500 μg/L（r=0.999 7—0.999 9）. The limits of detection are 0.002 5 μg/L and 0.005 μg/L，respectively. The recovery is in the range of 87.6%—98.2%, and the RSD is less than 3.5%．