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

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

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×1.7μm）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1.0~500.0μg/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 5μg/L和0.005μg/L,回收率为87.6%~98.2%,相对标准偏差小于3.5%。

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%.