固相萃取-同位素稀释-超高效液相色谱-串联质谱法测定水中涕灭威、涕灭威亚砜和涕灭威砜

Determination of Aldicarb,Aldicarb Sulfoxide,Aldicarb Sulfone in Water by Solid Phase Extraction and UPLC⁃MS/MS with Isotope Dilution

采用同位素稀释结合固相萃取对水样进行预处理,建立了环境水体中涕灭威及其代谢物(涕灭威亚砜、涕灭威砜)的超高效液相色谱-串联质谱分析方法。水样加同位素内标涕灭威-D_(3)、涕灭威亚砜-D_(3)和涕灭威砜-D_(3),经HLB固相萃取柱富集净化后,用Waters ACQUITY^(TM) BEH C18色谱柱(2.1 mm×100 mm,1.7μm)分离,以0.1%甲酸+5 mmol/L乙酸铵水溶液-乙腈为流动相,在电喷雾离子源正离子模式下进行多反应监测(MRM),内标法定量。3种目标化合物在0.5~200μg/L范围内线性良好,线性相关系数r≥0.999;方法检出限为0.0008~0.001μg/L,3个加标浓度水平的平均回收率为94.5%~108%,相对标准偏差为2.7%~6.5%。该方法采用了稳定同位素内标参与前处理的方法,消除了涕灭威降解对测定结果的影响,准确度好、灵敏度高,可用于环境水体中涕灭威及其代谢物涕灭威亚砜、涕灭威砜的测定。

A method for analysis of aldicarb,aldicarb sulfoxide and aldicarb sulfone in water was developed using solid phase extraction and HPLC-MS/MS with isotope dilution.The aqueous samples were spiked with isotope-labeled internal standards aldicarb-D_(3),aldicarb sulfoxide-D_(3) and aldicarb sulfone-D_(3),concentrated and purified on an HLB cartridge,and then separated on a Waters ACQUITY UPLC^(TM) BEH C_(18) column by gradient elution with 0.1%formic acid-5 mmol/L ammonium acetate-acetonitrile as the mobile phase.The analytes were detected by positive electrospray ionization with multiple reaction monitoring(MRM).The internal standard method was used to determine the results.There is a good linearity for target compounds in the range of 0.5~200μg/L with the correlation coefficient(r)larger than 0.999.The method detection limit(MDL)is 0.0008~0.001μg/L.The average recoveries range between 94.5%~105%at three different spiked levels.The relative standard deviation(RSD)is between 2.7%~6.5%.The method is sensitive and accurate,and is suitable for determination of aldicarb,aldicarb sulfoxide,aldicarb sulfone in water.