Novak Petra, Zuliani Tea, Milačič Radmila, Ščančar Janez
Department of Environmental Sciences, Jožef Stefan Institute, Jamova 39, Ljubljana 1000, Slovenia; Jožef Stefan International Postgraduate School, Jamova 39, Ljubljana 1000, Slovenia.
Department of Environmental Sciences, Jožef Stefan Institute, Jamova 39, Ljubljana 1000, Slovenia.
Anal Chim Acta. 2014 May 27;827:64-73. doi: 10.1016/j.aca.2014.04.020. Epub 2014 Apr 15.
Polybrominated diphenyl ethers (PBDEs) are flame retardants, which due to their widespread use are frequently present as pollutants in the environment. In the EU Water Framework Directive (WFD) six PBDE congeners (BDE 28, BDE47, BDE 99, BDE 100, BDE 153 and BDE 154) are listed as priority substances. The uncertainty of the analytical method used for their determination in water samples at environmental quality standard (EQS) level (0.5 ng L(-1) for the ΣPBDEs) should be equal or less than 50% and the limit of quantification (LOQ) for ΣPBDEs below 0.15 ng L(-1). To meet these requirements, an analytical procedure for the determination of these six PBDEs in environmental water samples by gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS) was developed. The acidification of water samples to pH 2 maintained the stability of PBDEs for at least 20 days. The use of Tris-citrate buffer enabled efficient desorption of PBDEs from suspended particulate matter (SPM) and humic acids (HA), and their further quantitative solvent extraction into 2 mL of iso-octane. When 300 mL of water sample was used for analysis and the organic phase concentrated to 25 μL, the expanded uncertainty for determination of PBDEs at EQS level was found to be around 40% (a coverage factor for a confidence level of 95%, k=2), and the LOQ for the ΣPBDEs 0.109 ng L(-1). Finally, to demonstrate the applicability of the newly developed GC-ICP-MS procedure, PBDEs were determined in river and sea water samples.
多溴二苯醚（PBDEs）是阻燃剂，由于其广泛使用，经常作为污染物存在于环境中。在欧盟水框架指令（WFD）中，六种多溴二苯醚同系物（BDE 28、BDE47、BDE 99、BDE 100、BDE 153和BDE 154）被列为优先物质。用于测定环境质量标准（EQS）水平（总多溴二苯醚为0.5 ng L⁻¹）水样中这些物质的分析方法的不确定度应等于或小于50%，总多溴二苯醚的定量限（LOQ）应低于0.15 ng L⁻¹。为满足这些要求，开发了一种通过气相色谱 - 电感耦合等离子体质谱法（GC - ICP - MS）测定环境水样中这六种多溴二苯醚的分析程序。将水样酸化至pH 2可使多溴二苯醚的稳定性保持至少20天。使用柠檬酸三缓冲液能够使多溴二苯醚从悬浮颗粒物（SPM）和腐殖酸（HA）中有效解吸，并将其进一步定量溶剂萃取到2 mL异辛烷中。当使用300 mL水样进行分析且有机相浓缩至25 μL时，发现测定EQS水平多溴二苯醚的扩展不确定度约为40%（置信水平为95%的包含因子，k = 2），总多溴二苯醚的LOQ为0.109 ng L⁻¹。最后，为证明新开发的GC - ICP - MS程序的适用性，对河水和海水样品中的多溴二苯醚进行了测定。
