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Analytical and Bioanalytical Chemistry

, Volume 397, Issue 1, pp 257–267 | Cite as

Determination of brominated diphenyl ethers (from mono- to hexa- congeners) in indoor dust by pressurised liquid extraction with in-cell clean-up and gas chromatography–mass spectrometry

  • María Pilar Martínez
  • José David Carrillo
  • María Teresa Tena
Original Paper

Abstract

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.

Keywords

Brominated diphenyl ethers Indoor dust Pressurised liquid extraction Gas chromatography Mass spectrometry In-cell clean-up 

Notes

Acknowledgements

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.

Supplementary material

216_2009_3333_MOESM1_ESM.pdf (556 kb)
ESM 1 (PDF 555 kb)

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Copyright information

© Springer-Verlag 2009

Authors and Affiliations

  • María Pilar Martínez
    • 1
  • José David Carrillo
    • 1
  • María Teresa Tena
    • 1
  1. 1.Department of ChemistryUniversity of La RiojaLogroñoSpain

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