Published:Journal of Chromatographic Science,
ISSN 0021-9665Volume
39, Number 10, October 2001, pp.
Preparation and Characterization of 3-(Aza-18-Crown-6) Propylsilyl
Bonded Phase for Reversed-Phase Liquid Chromatography
Shi-Lu Da, Yu-Qi Feng, Hui-Ning Da, Yin-Han Gong, and
Yuan-Wei Zhang
39,
Number 5, May 2001, pp. 200-204
Determination of
Diazinon, Chlorpyrifos, and Their Metabolites in Rat Plasma and Urine by High-Performance
Liquid Chromatography Aqel W. Abu-Qare and Mohamed B. Abou-Donia
Department of Pharmacology and Cancer Biology, Duke University Medical Center,
P.O. Box 3813, Durham, NC 27710
This
study reports a simple and rapid high-performance liquid chromatographic (HPLC)
method for the determination of the insecticide diazinon (O,O-diethyl-O[2-isopropyl-6-methylpyridimidinyl]
phosphorothioate), its metabolites diazoxon (O,O-diethyl-O-2-isopropyl-6-methylpyridimidinyl
phosphate) and 2-isopropyl-6-methyl-4-pyrimidinol, the insecticide chlorpyrifos
(O,O-diethyl-O[3,5,6-trichloro-2-pyridinyl] phosphorothioate) and its metabolites
chlorpyrifos-oxon (O,O-diethyl-O[3,5,6-trichloro-2-pyridinyl] phosphate), and
TCP (3,5,6-trichloro-2-pyridinol) in rat plasma and urine samples. The method
is based on using C18 Sep-Pak cartridges for solid-phase extraction and HPLC
with a reversed-phase C18 column and programmed UV detection ranging between
254 and 280 nm. The compounds are separated using a gradient of 1% to 80% acetonitrile
in water (pH 3.0) at a flow rate ranging between 1 and 1.5 mL/min in a period
of 16 min. The limits of detection ranged between 50 and 150 ng/mL, and the
limits of quantitation were 100 to 200 ng/mL. The average percentage recovery
of five spiked plasma samples were 86.3 ± 8.6, 77.4 ± 7.0, 82.1 ± 8.2, 81.8
± 8.7, 73.1 ± 7.4, and 80.3 ± 8.0 and from urine were 81.8 ± 7.6, 76.6 ± 7.1,
81.5 ± 7.9, 81.8 ± 7.1, 73.7 ± 8.6, and 80.7 ± 7.7 for diazinon, diazoxon, 2-isopropyl-6-methyl-4-pyrimidinol,
chlorpyrifos, chlorpyrifos-oxon, and TCP, respectively. The relationship between
the peak area and concentration was linear over a range of 200 to 2000 ng/mL.
This method was applied in order to analyze these chemicals and metabolites
following dermal administration in rats.
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