This study presents a selective pressurised liquid extraction (PLE) and gas chromatography–mass spectrometry/mass spectrometry method for the determination of brominated diphenyl ethers (BDEs) in indoor dust. Selective PLE consisted of the addition of Florisil mixed with the sample in order to perform an in-cell clean-up. This approach provided a cleaner and almost colourless extract, ready to be injected in the gas chromatograph. The PLE conditions were studied using an experimental design, firstly a 4 × 3 × 2 multifactor categorical design to screen sorbent, solvent and temperature and then a central composite design to optimise sorbent mass, temperature and time. Finally, the number of extraction cycles was studied. The selected conditions were 4 g of Florisil all mixed with the sample and no additional clean-up sorbent layer, 1:1 n-hexane-dichloromethane, 60% flush volume, 40 °C, 1,500 psi, 2-min static time and one cycle. The proposed method allowed accurate determination of BDEs, with recovery values between 82% and 101% and detection limits between 0.06 and 0.24 ng g−1. It also has advantages over other existing methods in terms of simplicity, automation, analysis time and solvent consumption.
Brominated diphenyl ethers Indoor dust Pressurised liquid extraction Gas chromatography Mass spectrometry In-cell clean-up
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The Spanish Ministerio de Educación y Ciencia, the Consejería de Educación, Cultura y Deportes of La Rioja and the University of La Rioja are thanked for supporting this work through the CTM2007-60404 project (within the Plan Nacional de Investigación Científica y Desarrollo e Innovación Tecnológica cofinanced with FEDER funds), the COLABORA 2008/06 project and the EGI08/41 project, respectively.