UPLC-MS/MS法测定饮用水中涕灭威及其代谢产物

建立了同时检测涕灭威、涕灭威砜和涕灭威亚砜的直接进样/超高效液相色谱/串联质谱(UPLC-MS/MS)方法。水样过膜后采用C18色谱柱分离,以10 mmol/L的甲酸铵水溶液和乙腈作为流动相进行梯度洗脱,采用多反应监测离子模式进行定性分析,外标法定量分析,线性范围分别在0. 5^50、0. 05^5和0. 1^10μg/L之间。在3个浓度添加水平下,涕灭威及其代谢产物的回收率为93. 5%^116. 2%,相对标准偏差为2. 3%^9. 4%。该方法的定量限为0. 04^0. 52μg/L。利用此方法连续3年跟踪调查了北京市市区主力水厂及其对应管网点的水质情况,结果表明北京市市区供水中不存在涕灭威及其代谢产物污染风险。

Determination of Aldicarb and Its Metabolites in Drinking Water by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry

A method was developed for the determination of aldicarb and its metabolites in drinking water by using ultra high performance liquid chromatography-tandem mass spectrometry (UPLCMS/MS). Water samples were separated by C18 column after membrane filtration. Aldicarb,aldicarb sulfone and aldicarb sulfoxide were separated through a reversed phase column according to a gradient elution program with 10 mmol/L ammonium formate aqueous solution and acetonitrile solution as mobile phase. Qualitative analysis was performed using multiple-reaction monitoring (MRM). The linear range of calibrations of aldicarb,aldicarb sulfone and aldicarb sulfoxide were 0. 5-50 μg/L,0. 05-5 μg/L and 0. 1-10 μg/L,respectively. The recoveries were in a range of 93. 5%-116. 2%,and their relative standard deviations (RSDs) were 2. 3%-9. 4% at three spiked levels for all analytes. The limits of quantification (LOQ) for aldicarb and its metabolites were between 0. 04 μg/L and 0. 52 μg/L.Based on this method,drinking water samples from the main water treatment plants and their control stations in Beijing were analyzed for three years. Results showed that no pollution risk of aldicarb and its metabolites was found in the urban water supply of Beijing.