水中呋喃丹及5种有机磷农药的超高效液相色谱串联质谱测定法

Determination of carbofuran and five organophosphorus pesticides in water by UPLC-MS/MS

目的建立高效、准确测定水中呋喃丹及5种有机磷农药的方法。方法 100 ml水样经固相萃取前处理,0.2μm滤膜过滤后,以Acquity UPLC BEH C18（2.1 mm×100 mm,1.7μm）为分析柱,0.2%甲酸和乙腈为流动相,采用正离子扫描多反应监测模式检测。结果乐果在0.9-2 000 ng/L,敌敌畏在2.5-5 000 ng/L,呋喃丹在0.6-2 000 ng/L,甲基对硫磷在19-5 000 ng/L,马拉硫磷在0.9-5 000 ng/L,毒死蜱在0.8-5 000 ng/L浓度范围内,线性关系良好,r〉0.999,方法检出限为0.6-19 ng/L,回收率为89.6%-129%,RSD〈11%。结论该方法高效、准确、灵敏度高,选择性好,适用于地表水及生活饮用水中上述6种农药的测定。

Objective To establish a method of purge and trap in combination with gas chromatography-mass spectrometry（PT-GC/MS） for the determination of nine halogenated hydrocarbons（1,2-dibromoethane,1,2-dibromoethene,trichloroethane,carbon tetrachloride,trichloroethylene,tetrachloroethylene,bromodichloromethane,dibromomonochloromethane,tribromomethane） in drinking water simultaneously.Methods Nine halogenated hydrocarbons in drinking water were concentrated by purge and trap,and then analyzed with capillary column,determined by MS detector.Results The linear range of 1,2-dibromoethene was0.01-0.93 μg/L,of other eight component were 0.01-0.80 μg/L.The limit of detection（LOD） were 0.002-0.004 μg/L.The recovery rates were 84.4%-106%.The relative standard deviations（RSD） were 1.0%-8.9%.Conclusion For its high sensitivity,good repeatability,simple operation and solvent-free,this method is applicable to the determination of nine halogenated hydrocarbons in drinking water.