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Analysis of polybrominated diphenyl ethers (PBDEs) by liquid chromatography with negative-ion atmospheric pressure photoionization tandem mass spectrometry (LC/NI-APPI/MS/MS): application to house dust

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Abstract

Eight polybrominated diphenyl ether (PBDE) congeners of primary interest to the US EPA were separated using reverse-phase liquid chromatography on an octadecylsilane column. BDE-28, BDE-47, BDE-99, BDE-100, BDE-153, BDE-154, BDE-183, and BDE-209 were baseline-resolved under isocratic conditions in 92:8 methanol/water (v/v). Negative-ion atmospheric pressure photoionization (NI-APPI) with a toluene dopant produced precursor ions corresponding to [M–Br+O]– for the eight congeners studied. Each congener was quantified by tandem mass spectrometry through a unique multiple reaction monitoring (MRM) transition. On-column limits of detection were between 2.4 and 27.8 pg for the eight congeners studied, with an intra-day method precision of 9%. The LC/NI-APPI/MS/MS method was validated for the analysis of the eight PBDE congeners in NIST SRM 2585 (Organics in House Dust). Pressurized liquid extraction (PLE) with subsequent LC/NI-APPI/MS/MS analysis afforded quantitative recovery for all eight PBDE congeners with recoveries ranging from 92.7 to 113%. The liquid-phase separation of the LC/NI-APPI/MS/MS method is not prone to the thermal degradation issues that plague splitless GC based analyses of highly brominated PBDEs such as BDE-209.

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Acknowledgments

We are grateful to Michelle Schantz at NIST for providing SRM 2585. This material is based upon work supported by the National Science Foundation under grant numbers CHE-0718530 and CHE-0619394.

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Authors and Affiliations

  1. Department of Chemistry, Villanova University, 800 Lancaster Avenue, Villanova, PA, 19085–1699, USA

    Anthony F. Lagalante & Timothy D. Oswald

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  1. Anthony F. Lagalante
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  2. Timothy D. Oswald
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Correspondence to Anthony F. Lagalante.

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Lagalante, A.F., Oswald, T.D. Analysis of polybrominated diphenyl ethers (PBDEs) by liquid chromatography with negative-ion atmospheric pressure photoionization tandem mass spectrometry (LC/NI-APPI/MS/MS): application to house dust. Anal Bioanal Chem 391, 2249–2256 (2008). https://doi.org/10.1007/s00216-008-2156-z

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  • DOI: https://doi.org/10.1007/s00216-008-2156-z

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