Analytical and Bioanalytical Chemistry

, Volume 391, Issue 6, pp 2249–2256

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

Original Paper

DOI: 10.1007/s00216-008-2156-z

Cite this article as:
Lagalante, A.F. & Oswald, T.D. Anal Bioanal Chem (2008) 391: 2249. doi:10.1007/s00216-008-2156-z

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.

Keywords

Negative-ion atmospheric pressure photoionization (NI-APPI) Liquid chromatography tandem mass spectrometry (LC/MS/MS) Dust Polybrominated diphenyl ethers (PBDEs) Pressurized liquid extraction (PLE) 

Copyright information

© Springer-Verlag 2008

Authors and Affiliations

  1. 1.Department of ChemistryVillanova UniversityVillanovaUSA

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