建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法同时测定污水中14种有机磷酸酯阻燃剂(OPEs)的分析方法.样品采集后,经GF/C膜过滤,HLB固相萃取小柱净化后进样分析.以BEH C18色谱柱为分离柱,乙腈和水混合液为流动相(0.2 mL min^-1)梯度洗脱,15 min内可完成14种OPEs的分离.在电喷雾正离子模式下,采用多反应监测模式(MRM)进行质谱测定.在加标浓度为1.0μg·L^-1时,14种OPEs在污水处理厂进水和出水中的回收率分别为52.1%—119%、43.6%—114%,相对标准偏差(RSD)分别为1.2%—16.2%、0.4%—9.2%,方法的检出限(LOD)在0.3—6.0 ng·L^-1间.方法精密度好,准确度高,可满足同时对污水样品中的14种OPEs进行定性及定量分析的要求.
An ultra-performance liquid chromatography-tandem mass spectrometry( UPLC-MS /MS)method was developed for the simultaneous determination of 14 organophosphate esters( OPEs) in waste water. The collected water samples were filtered with GF /C membrane and purified by solid phase extraction( SPE) using HLB cartridges. The eluent was collected and concentrated to nearly drieness under a gentle stream of nitrogen gas,and then re-dissolved with 1 mL initial mobile phase( 40%( V/V) acetonitrile in water) and analyzed by UPLC-MS/MS under positive electrospray ionization and multiple reaction monitoring( MRM). Separation of analytes was finished in 15 min by using a BEH C18 column,and gradient elution with a mixture of acetonitrile and water as mobile phases( 0. 2 mL·min^-1). The recoveries of all the compounds from the influent water and effluent water of a wastewater treatment plant,at the spiked concentration levels of 1. 0 μg·L^-1,were respectively in the range of 52. 1% —119% and 43. 6% —114%,with the corresponding relative standard deviations( RSD) of 1. 2% —16. 2% and 0. 4% —9. 2%. The method detection limits ranged from 0. 3 to 6. 0 ng·L^-1. The method could be applied in the analysis of 14 OPEs in waste water samples with good precisions and accuracies.