Published:Journal of Chromatographic Science,
ISSN 0021-9665 Volume 44,
Number 8, September 2006, pp. 489-497
Comparison of Analytical Strategies for the Chromatographic
and Mass Spectrometric Measurement of Brominated Flame Retardants:
1. Polybrominated Diphenylethers
Ronan Cariou[1], Jean-Philippe Antignac[1], Laurent
Debrauwer[2], Daniel Maume[1], Fabrice Monteau[1], Daniel Zalko[2],
Bruno le Bizec[1], and François Andre[1]
[1]Laboratoire d’Etude des Résidus et Contaminants
dans les Aliments (LABERCA), Ecole Nationale Vétérinaire
de Nantes (ENVN), Unité Sous Contrat INRA (Institut National
de la Recherche Agronomique), BP 50707, 44307 Nantes cedex 3 and
[2]UMR 1089 Xénobiotiques, Institut National de la Recherche
Agronomique, BP3, 31931 Toulouse cedex 9, France
The chromatographic and mass spectrometric (MS)
behaviors of 49 polybrominated diphenylether (PBDE) homologues
toward various techniques is investigated. Special attention is
paid to chromatographic separation, ionization processes, and
signal acquisition modes. Different liquid chromatographic (LC)
separation systems and gas chromatographic (GC) temperature program
parameters are studied. For LC–MS experiments, the ionization
efficiencies of electrospray, atmospheric pressure chemical ionization,
and atmospheric pressure photoionization (APPI) are evaluated.
For GC–MS experiments, negative chemical ionization with
ammonia as reagent gas as well as negative and positive electron
impact (EI) ionization are studied. Thus, fragmentation pathways
of PBDEs are investigated, with the main objective being to determine
the sensitivity/specificity balance of each tested technique with
respect to their potential respective application (parent compound
focusing, metabolite identification, and screening of analogue
compounds). Finally, performances of the different tested techniques
are compared and evaluated in terms of detection limits on standard
solutions for each homologue group. In terms of ionization, EI
remains the best compromise between sensitivity and specificity
with possible complementary applications in MS–MS and high-resolution
MS. Nevertheless, APPI appears to be a promising alternative.
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