液相色谱-串联四极杆质谱法测定海水和海底泥中的有机磷酸酯类阻燃剂
Determination of organophosphate ester flame retardants in seawater and sediments by liquid chromatography-tandem quadrupole mass spectrometry
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摘要: 本文建立了基于液相色谱串联四极杆质谱联用技术同时测定海水和海底泥中26种常见有机磷酸酯类（OPEs）阻燃剂的方法.海水中的OPEs经过极性修饰的聚合物反相固相萃取Bond Elut PPL柱富集和净化，采用同位素稀释法进行定量.在0.5—100 ng·L-1浓度范围内，大部分OPEs的线性响应良好，回归系数大于0.99.海水中OPEs检测方法检出限在0.0003—26.0 ng·L-1，3个添加水平下添加回收率和相对标准偏差分别在51.8%—123.0%和0.7%—13.6%之间；海底泥中OPEs方法检出限在0.0001—0.02 μg·kg-1之间，添加回收率和相对标准偏差分别在52.1%— 118.1%和1.5%—12.0%之间，结果表明，该方法灵敏、准确、可靠，可以满足环境海水与海底泥样品中痕量OPEs的检测要求.Abstract: A method was developed for the simultaneous determination of 26 common organophosphate esters (OPEs) flame retardants in seawater and sediments by liquid chromatography tandem quadrupole mass spectrometry. The OPEs in seawater were enriched and purified by the polar-modified polymer reversed-phase solid phase extraction, Bond Elut PPL column, and quantified by the isotope dilution method. The method delivered excellent linearity for most OPEs over the range of 0.5—100 ng·L-1, with linear regression coefficients higher than 0.99. The detection limits of OPEs in seawater ranged from 0.0003 ng·L-1 to 26.0 ng·L-1, and the recoveries ranged from 51.8% to 123.0% at low, medium and high spiked levels with relative standard deviations (RSDs) within 0.7 to 13.6%, respectively. The detection limits of OPEs in sediments ranged from 0.0001 μg·kg-1 to 0.02 μg·kg-1, and the recoveries ranged from 52.1% to 118.1% respectively with RSDs within 1.5% to 12.0%. The results show that the method is sensitive, accurate and reliable, and can meet the requirements for the determination of trace OPEs in environmental seawater and sediments samples.
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