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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 32, Number 4, May,
pp.303-307
Determination
of p-tert-Octylphenol in Blood and Tissues by Gas Chromatography
Coupled with Mass Spectrometry
G. Hamelin1, G. Charest-Tardif1, K. Krishnan1, D.G. Cyr2, M. Charbonneau2,
P.J. Devine2, S. Haddad3, G.M. Cooke4,5, T. Schrader4, and R. Tardif1,
1Département de santé environnementale et santé au
travail, Université de Montréal, Montréal,
Québec, Canada;
2INRS-Institut Armand-Frappier, Institut
national de la recherche scientifique, Pointe Claire, Québec,
Canada;
3Département des sciences biologiques. Université du
Québec à Montréal, Montréal, Québec,
Canada;
4Toxicology Research Division, Bureau of Chemical Safety,
Food Directorate, Health Products and Food Branch, Health Canada,
Sir Frederick G. Banting Research Centre, Tunney’s Pasture,
Ottawa, Ontario, Canada;
5Departments of Cellular and Molecular
Medicine and Obstetrics and Gynecology, University of Ottawa, Ottawa,
Ontario, Canada
A sensitive and reproducible procedure using gas
chromatography coupled with mass spectrometry is described for
the determination of p-tert-octylphenol (OP), a persistent
degradation product of alkylphenol ethoxylates that binds to
the estrogen receptor in blood and tissues. The first step involved
the extraction of blood (200 µL) or tissue homogenate (400 µL)
with methyl tert-butyl ether, including p-tert-butylphenol
(BP) as internal standard. After extraction, the sample was evaporated
to dryness with a gentle stream of nitrogen at 45°C, and
OP and BP were derivatized with an acetylation reaction involving
acetic anhydride and catalyzed by pyridine. Samples were then
analyzed by a gas chromatograph equipped with a mass spectrometer
(single ion monitoring) with a Varian VF-5ms capillary column.
The limit of detection and the limit of quantification of the
method in blood were 4.6 and 15.5 ng/mL, respectively. The linearity
and reproducibility of the method were acceptable, with coefficients
of variation of approximately 10% for blood and ranging between
9% and 27% for tissues. This method was applied to the determination
of unchanged OP in blood and tissues obtained from Sprague-Dawley
rats after oral and IV OP administration.
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