Toxicological Center, University of Antwerp, Universiteitsplein 1, 2610 Wilrijk-Antwerp, Belgium.
Environ Int. 2011 Feb;37(2):454-61. doi: 10.1016/j.envint.2010.11.010. Epub 2010 Dec 21.
A new and efficient analytical method was developed and validated for the analysis of organophosphorus flame retardants (OPFRs) in indoor dust samples. This method involves an extraction step by ultrasonication and vortex, followed by extract clean-up with Florisil solid-phase extraction cartridges and analysis of the purified extracts by gas chromatography-mass spectrometry (GC-MS). Method recoveries ranged between 76 and 127%, except for volatile OPFRs, such as triethyl phosphate (TEP) and tri-(n-propyl) phosphate (TnPP), which were partially lost during evaporation steps. The between day precision on spiked dust samples was <14% for individual OPFRs, except for TEP, tri-iso-butyl phosphate (TiBP) and tri (2-butoxyethyl) phosphate (TBEP). Method limit of quantifications (LOQ) ranged between 0.02 μg/g (TnPP and tris(1-chloro-2-propyl phosphate (TCPP)) and 0.50 μg/g (TiBP). The method was further applied for the analysis of indoor dust samples taken from Flemish homes and stores. TiBP, TBEP and TCPP were most abundant OPFR with median concentrations of 2.99, 2.03 and 1.38 μg/g in house dust and of 1.04, 3.61, and 2.94 μg/g in store dust, respectively. The concentration of all OPFRs was at least 20 to 30 times higher compared to polybrominated diphenyl ethers (PBDEs) and hexabromocyclododecanes (HBCDs). Estimated exposure to OPFRs from dust ingestion ranged for individual OPFRs between <1 and 50 ng/kg body weight for adults and toddlers, respectively. The estimated body burdens were 1000 to 100 times below reference dose (RfD) values, except for the scenario with high dust ingestion and high concentrations of TBEP in toddlers, where intake was only 5 times below RfD. Exposure of non-working and working adults to OPFRs appeared to be similar, but in specific work environments, exposure to some OPFRs (e.g. TDCPP) was increased by a factor >5.
开发并验证了一种新的、高效的分析方法,用于分析室内灰尘样品中的有机磷阻燃剂 (OPFRs)。该方法包括超声和涡旋提取步骤,然后用 Florisil 固相萃取小柱进行提取净化,最后用气相色谱-质谱法 (GC-MS) 分析净化提取物。方法回收率在 76%至 127%之间,除了挥发性 OPFRs 如三乙基磷酸酯 (TEP) 和三正丙基磷酸酯 (TnPP) 外,它们在蒸发步骤中部分损失。在添加灰尘样品中,除 TEP、三异丁基磷酸酯 (TiBP) 和三 (2-丁氧基乙基) 磷酸酯 (TBEP) 外,个别 OPFR 的日内精密度<14%。方法定量限 (LOQ) 范围为 0.02 μg/g (TnPP 和三氯 (1- 丙基) 磷酸酯 (TCPP)) 和 0.50 μg/g (TiBP)。该方法进一步应用于从佛兰芒家庭和商店采集的室内灰尘样品的分析。TiBP、TBEP 和 TCPP 是最丰富的 OPFR,在家庭灰尘中的中位数浓度分别为 2.99、2.03 和 1.38 μg/g,在商店灰尘中的中位数浓度分别为 1.04、3.61 和 2.94 μg/g。所有 OPFR 的浓度至少比多溴二苯醚 (PBDEs) 和六溴环十二烷 (HBCDs) 高 20 至 30 倍。通过灰尘摄入估计的 OPFR 暴露量,对于成年人和幼儿,个别 OPFR 的范围分别为<1 至 50 ng/kg 体重。估计的体负荷比参考剂量 (RfD) 值低 1000 至 100 倍,除了幼儿高灰尘摄入和 TBEP 浓度高的情况下,摄入量仅比 RfD 值低 5 倍。非工作和工作成年人接触 OPFRs 的情况似乎相似,但在特定的工作环境中,一些 OPFRs(如 TDCPP)的暴露量增加了 5 倍以上。