Extraction and cleanup of fish, sediment, and water for determination of triaryl phosphates by gas-liquid chromatography.

Several techniques were evaluated for extracting triphenyl phosphate (TPP), 14C-labeled TPP, cresyl diphenyl phosphate, and tricresyl phosphate isomers (o-TCP, m-TCP, and p-TCP) from fish and sediment samples. Extracts of fish samples were cleaned up by gel permeation chromatography/alumina column chromatography; sediment extracts received alumina treatment only. Compounds were determined by gas-liquid chromatography (GLC) with nitrogen-phosphorus detection. Methanol/Polytron and hexane/ball mill extraction of fish samples fortified at 0.01, 0.1, and 1.0 microgram/g levels gave overall recoveries of the 5 compounds of 89 and 97%, respectively. Methanol recovered more radioactivity (97%) from fish exposed to 14C-TPP in aquaria for 24 h than did hexane from fish exposed for 16 h (79%). Refluxing fortified sediment (0.05 and 0.5 microgram/g) with methanol-water (9 + 1) gave significantly higher recoveries (88%) of the 5 triaryl phosphates than did dichloromethane-methanol (1 + 1) reflux or acetone-hexane (1 + 1) Soxhlet extraction. Recoveries of TPP and o-, m- and p-TCP from fortified river water (0.5, 5.0, and 50 microgram/L) by shaking with dichloromethane ranged from 91 to 118%. Some problems were encountered with interfering GLC peaks at low (microgram/g) levels in fish and sediment extracts despite the use of nitrogen-phosphorus specific detectors.