Solid-phase extraction and purification for the quantification of polycyclic aromatic hydrocarbon metabolites in fish bile |
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Authors: | Olivier?Mazéas Email author" target="_blank">Hélène?BudzinskiEmail author |
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Institution: | (1) Laboratoire de Physico-et Toxico-Chimie des Systèmes Naturels, UMR 5472 CNRS, Université Bordeaux I, 351, cours de la libération, 33405 Talence, France |
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Abstract: | An analytical protocol including solid-phase extraction and purification is described for the individual quantification of
polycyclic aromatic hydrocarbon metabolites (hydroxylated PAHs) in liquid biological matrices such as plasma and bile. The
method consists in an enzymatic deconjugation followed by a solid-phase extraction on a C18 cartridge and by a cleanup on an NH2 cartridge. Extracts are then submitted to a derivatization step before gas chromatography/mass spectrometry (GC/MS) analysis.
The quantification of PAH metabolites is ensured by adding an internal standard, 1-hydroxypyrene deuterated, at the beginning
of the protocol. Recoveries obtained for the entire protocol were for the major part of the compounds between 96 and 70%.
However, recoveries were not so satisfying concerning 2-hydroxybiphenyl and especially 3-hydroxybenzo(a)pyrene, with 62 and
36% respectively. Finally, the protocol was applied to different fish bile samples and showed its good applicability to fish
bile samples. The NH2 cleanup step has been proved to be a very selective purification step, necessary to remove most of the bile pigments before
GC/MS injection. Different PAH metabolites could be detected in those natural samples and their quantification allowed us
to distinguish different levels of fish exposure. |
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Keywords: | Hydroxylated polycyclic aromatic hydrocarbons Solid-phase extraction Purification Gas chromatography/mass spectrometry Fish bile Metabolites |
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