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Published:
Journal of Analytical Toxicology,
ISSN 0146-4760,
Volume 24,
Number 8, November/December,
pp.678-684
Determination of
Dialkyl Phosphates in Human Urine using Gas Chromatography–Mass Spectrometry
Jochen
Hardt and Jürgen Angerer*
Institute and Outpatient Clinic of Occupational, Social, and Environmental Medicine
of the University of Erlangen-Nürnberg, Schillerstraße 25, D-91054
Erlangen, Germany
Organophosphates
are used as pesticides in agriculture and pest control. They are metabolized
to dialkylphosphates, which are excreted in urine. Determination of these metabolites
is useful for assessing human exposure to organophosphates. This publication
describes a new, reliable, and very sensitive analytical procedure for quantitating
dimethylphosphate (DMP), diethylphosphate (DEP), O,O-dimethylthiophosphate (DMTP),
O,O-diethylthiophosphate (DETP), O,O-dimethyldithiophosphate (DMDTP), and O,O-diethyldithiophosphate
(DEDTP) in human urine. The analytes are extracted from acidified urine into
a mixture of diethylether and acetonitrile. Dibutylphosphate serves as internal
standard. Derivatization is performed using pentafluorobenzylbromide at 40°C
overnight. After further liquid–liquid extraction, analysis is carried
out by gas chromatography–mass spectrometry. The limits of detection are
5 µg/L urine for DMP and 1 µg/L for the other five metabolites.
Using the new procedure, 54 spot urine samples from persons in the general population
in Germany were analyzed. Nearly every sample contained DMP, DEP, and DMTP,
and the median values (95th percentiles) of the concentrations were 30 µg/L
(105 µg/L), 4 µg/L (21 µg/L), and 22 µg/L (174 µg/L),
respectively. DETP and DMDTP were found in lower concentrations. Reproduction
of editorial content of this journal is prohibited without publisher’s
permission.
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