A simple method using direct sample injection combined with liquid chromatography tandem mass spectrometry has been developed for the simultaneous analysis of six alkaloid compounds in environmental samples. The target list includes two psychostimulants (nicotine and caffeine), three metabolites (cotinine, nicotinic acid and paraxanthine) and a coffee chemical (trigonelline). The analytical method was evaluated in three different matrices (surface water, influent and effluent wastewater). The method developed showed an adequate sensitivity, below 0.6 μg L(-1) for wastewater and 0.1 μg L(-1) for river matrices, without any prior treatment of the samples. Finally, the methodology was applied to real samples for evaluation of their removal from a sewage treatment plant and their persistence/fate in the aquatic environment. All compounds studied in this work were detected at all sampling points collected along the Henares River. However, nicotinic acid was only detected three times in treated sewage samples at levels above its detection limit.
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