Toxicological Center, University of Antwerp, Universiteitsplein 1, 2610 Wilrijk, Antwerp, Belgium.
Talanta. 2012 Jan 30;89:292-300. doi: 10.1016/j.talanta.2011.12.031. Epub 2011 Dec 19.
A new method was optimized for the simultaneous determination of several flame retardants (FRs) in indoor dust, namely polybrominated diphenyl ethers (PBDEs), hexabromocyclododecanes (HBCDs), novel brominated flame retardants (NBFRs) and organophosphate ester flame retardants (OPFRs). The method was based on two previously validated analytical methods for NBFRs and OPFRs, which were combined in order to include even a large number of FRs. An ultrasonic extraction method and two-stage clean-up by adsorption chromatography was optimized using an indoor dust standard reference material (SRM 2584). The 1st cleanup step was essential for fractionation of analytes in the dust extracts, while the 2nd step was important for the further removal of interferences. Analysis of cleaned dust extracts was performed with gas chromatography electron impact ionization mass spectrometry for OPFRs, gas chromatography electron capture negative ionization mass spectrometry for PBDEs and NBFRs and liquid chromatography electrospray ionization tandem mass spectrometry for HBCDs. Method validation by matrix spiking demonstrated good accuracy ranging from 81 to 130%. Matrix effects were investigated by spiking sodium sulfate and dust with analyte standards. Typical recoveries ranged between 80 and 110% at both spiking levels, though occasional deviations were observed at low spiking concentrations. Precision between different days was generally below 24% relative standard deviation (RSD) at low concentrations and below 11% RSD at high concentrations. Method limits of quantification for BFRs ranged between 0.04 (BDE 28) and 17 ng/g (BDE 209), 6 ng/g for sum HBCDs, and for OPFRs between 10 (triphenyl phosphate) and 370 ng/g (tri-isobutyl phosphate). The method was applied to SRM 2585 and to a set of indoor dust samples from various countries. The newly developed method will be employed for the monitoring of human exposure via dust ingestion to phased-out and alternate FRs.
优化了一种新方法，用于同时测定室内灰尘中的几种阻燃剂（FRs），即多溴二苯醚（PBDEs）、六溴环十二烷（HBCDs）、新型溴化阻燃剂（NBFRs）和磷酸酯阻燃剂（OPFRs）。该方法基于先前为 NBFRs 和 OPFRs 验证的两种分析方法，将其组合在一起以包含大量 FRs。采用室内灰尘标准参考物质（SRM 2584）对超声提取方法和吸附色谱两级净化进行了优化。第一步净化对于灰尘提取物中分析物的分离至关重要，而第二步对于进一步去除干扰物非常重要。用气相色谱电子轰击电离质谱法分析经净化的灰尘提取物，用气相色谱电子俘获负电离质谱法分析 PBDEs 和 NBFRs，用液相色谱电喷雾串联质谱法分析 HBCDs。基质加标验证表明，方法的准确度良好，范围为 81%至 130%。通过向硫酸钠和灰尘中添加分析物标准品来研究基质效应。在两种添加水平下，典型回收率在 80%至 110%之间，但在低添加浓度下偶尔会出现偏差。在低浓度下，不同天之间的精密度通常低于 24%相对标准偏差（RSD），在高浓度下低于 11%RSD。BFRs 的方法定量限在 0.04（BDE 28）至 17ng/g（BDE 209）之间，HBCDs 的总和为 6ng/g，OPFRs 的方法定量限在 10（三苯基磷酸酯）至 370ng/g（三异丁基磷酸酯）之间。该方法应用于 SRM 2585 和来自不同国家的一系列室内灰尘样品。新开发的方法将用于通过灰尘摄入监测人类对淘汰和替代 FRs 的暴露情况。
