气相色谱-串联质谱法测定沉积物中有机磷酸酯

Analysis of Organophosphate Esters in Sediment Samples Using Gas Chromatography-Tandem Mass Spectrometry

比较了不同提取方法、净化方法对沉积物样品中有机磷酸酯（Organophosphate esters,OPEs）的富集、净化效果,建立了气相色谱-串联质谱法（GC-MS/MS）检测沉积物中8种OPEs的分析方法。用20 m L正己烷-丙酮混合液（1∶1,V/V）、涡流振荡＋超声提取两次,Florisil固相萃取柱净化、8 m L乙酸乙酯洗脱,浓缩后将溶剂置换成正己烷,采用DB-5MS毛细管柱（30 m×0.25 mm×0.25μm）进行分离,质谱检测器在选择反应监测模式（SRM）下进行分析,内标法定量。结果表明,此前处理方法操作简单、溶剂耗量少;在3个添加浓度水平下,OPEs（除TEP外）的回收率在80%~120%之间,检出限为0.31~65 ng/L,且有良好的精密度与准确度。

An efficient extraction and purifying method coupled to gas chromatography-tandem mass spectrometry （GC-MS/MS） with electron impact （E1） detection was developed to determine eight organophosphate esters （OPEs） in sediment samples. The selected OPEs were extracted twice from the sediments through vortex oscillation and ultrasonic extraction using 20 mL of n-hexane and acetone mixture （1：1, V/V） for 10 min. Further purification by Florisil solid phase extraction （SPE） column, elution by 8 mL of ethyl acetate, concentration, and solvent exchanges for n-hexane were carried out. All target compounds were separated using the DB-5ms capillary column （30 m × 0.25 mm × 0.25 μm） and detected by tandem mass spectrometry with selected reaction monitoring, and determined by the internal standard method. The result showed that this pretreatment method was simple with less solvent consumption. At three spiked levels of 10, 20 and 50 μg/L, the recovery of selected OPEs （except TEP） was 80% to 120%, and the limit of detection was 0.31-64.5 ng/L, showing a good precision and accuracy.