A method is described for the determination of triethylamine in environmental samples such as river water and bottom sediment. Triethylamine was distilled from an environmental sample under basic condition, extracted under. The same condition with diethylether, and determined by capillary gas chromatography-selected-ion-monitoring (GC-SIM) . The detection limits from river water and bottom sediment were 0.15 μg/1 and 0.94 μg/kg, respectively. The recoveries from river water and bottom sediment were over 80% with coefficient of variation below 4%. This method have sufficient sensitivity, selectivity, and accuracy to be applicable to environmental samples.