液相色谱串联质谱法直接测定地下水中痕量呋喃丹、涕灭威及其代谢物

Trace Determination of Carbofuran,Aldicarb and Its Metabolites in Groundwater by LC-MS/MS with Direct Injection

建立了直接进样液相色谱-电喷雾串联质谱(LC-MS/MS)测定地下水中呋喃丹、涕灭威及其代谢物涕灭威亚砜和涕灭威砜的分析方法。对质谱条件和液相色谱条件进行了优化,以甲醇-水为流动相,多反应监测模式(MRM)对目标物进行定性定量分析。结果表明:目标物在0.05～100μg/L范围内线性关系良好,相关系数(r2)为0.996 0～0.999 3;方法检出限为0.01～0.05μg/L;以3个水平进行样品加标实验,目标化合物的回收率为90%～106%,相对标准偏差(RSD,n=8)为2.7%～6.5%。该方法定性定量准确,灵敏度高,避免了复杂的样品前处理过程,可用于地下水中痕量氨基甲酸酯农药的测定。

A method was established for the determination of carbofuran, aldicarb and its metabolite in groundwater by liquid chromatography - electrospray ionization tandem mass spectrometry with direct injection. The optimization conditions of LC and MS were discussed. Methanol and water were chosen as mobile phase. Under the optimal conditions, the calibration curves for carbamate and its metabolite were linear in the range of 0.05 - 100 μg/L, with correlation coefficients between 0. 996 0 and 0. 999 3. The limits of detection（S/N≥5） were between 0. 01 μg/L and 0.05 μg/L. The recoveries of target compounds at three spiked concentration levels ranged from 90% to 106% with relative standard deviations（RSDs, n = 8）of 2.7% -6.5%. This method was accurate and sensitive, and was suitable for the trace determination of carbamate in groundwater.