玉米中9种磺酰脲类除草剂的超高效液相色谱-串联质谱法同时测定

采用超高效液相色谱-串联四极杆质谱(UPLC-MS/MS),在多反应监测(MRM )模式下建立了玉米中9种磺酰脲类除草剂残留的定性定量分析方法.样品浸泡后采用甲醇-丙酮(体积比1:1)提取、浓缩,经C18固相萃取柱净化处理.采用UPLC-ESI MS/MS方法测定,外标法定量.9种磺酰脲类除草剂在0.05～2.0 mg...

Simultaneous Determination of 9 Sulfonylurea Herbicides in Corn Using Solid phase Extraction and Ultra Performance Liquid Chromatography with Electrospray Ionization Tandem Mass Spectrometry

A new method based on solid phase extraction and ultra performance liquid chromatography-tandem mass spectrometry(UPLC-ESI MS/MS) was developed for the determination of 9 sulfonylurea herbicides(metoxuron,foramsulfuron,cinosulfuron,methabenthiazuron,prosulfuron,linuron,ethoxysulfuron,chloroxuron and cyclosulfamuron) in corn.The corn sample was soared in water,and then extracted with methanol-acetone(1∶1,by volume).The extract was cleaned up by C18 solid phase extraction cartridge.The eluent was evaporated to near dryness under a stream of nitrogen gas,and redissolved by methanol.The identification and detection of target compounds were achieved under multiple reactions monitoring(MRM)mode with positive electrospray ionization(ESI).9 sulfonylurea herbcides were quantified by external standard method.The calibration curves of 9 sulfonylurea herbicides were linear in the range of 0.05-2.0 mg·L-1 with correlation coefficients more than 0.99.The limits of detection(LOD,S/N=3) and the limits of quantitation(LOQ,S/N=10) were in the range of 0.001-0.005 mg·L-1 and 0.062-0.080 mg·kg-1,respectively.1LOQ,2LOQ and 5LOQ were chosen as the three spiked levels of recovery for the method.The recoveries of 9 sulfonylurea herbicides ranged from 60% to 85% with relative standard deviations less than 10%.The method was simple and effective,and could meet the requirements the simultaneous determination of 9 sulfonylurea herbicides in corn sample.