Published: Journal of Analytical Toxicology, Volume 22, Number 3, May/June 1998, pp. 248–252.

CASE REPORT: Analysis of Fenthion in Postmortem Samples by HPLC with Diode-Array Detection and GC–MS Using Solid-Phase Extraction,
E. Meyer, D. Borrey, W. Lambert, C. Van Peteghem, M. Piette, and A. De Leenheer

Fenthion (O,O-dimethyl-O-[3-methyl-4-(methylthio)-phenyl]-thiophosphate) is an organophosphate insecticide. A specific method to quantitate fenthion in postmortem matrices with solid-phase extraction combined with high-performance liquid chromatography–diode-array detection (HPLC–DAD) and gas chromatography–mass spectrometry (GC–MS) is presented. Fenitrothion (O,O-dimethyl-O-[3-methyl-4-nitrophenyl]-thiophosphate) is selected as the internal standard. For sample cleanup, a simple but selective solid-phase extraction is chosen after comparison with traditional liquid–liquid extraction procedures. Homogenized and appropriately diluted aqueous samples are applied, and the analytes are desorbed with 5 mL of dichloromethane. Aliquots of the extract are used for HPLC–DAD and GC–MS analysis. Liquid and GC conditions are as follows: gradient elution with a mixture of methanol and water (10:90 to 90:10, v/v) containing 0.0125M NaOH on an Aluspher RP-Select B column monitoring at 250 nm, and temperature programming from 60 to 300°C on a dimethylpolysiloxane column in the SCAN mode, respectively. This method is applied to a suicidal case involving unsuspected acute intoxication with fenthion (concentration in blood, 3.8 µg/mL).

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