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Ultraperformance liquid chromatography coupled to electrospray tandem mass spectrometry was used for the rapid and simultaneous analysis of 15 stimulatory drugs in water. Cocaine, amphetamine-related compounds, LSD, ketamine, PCP, fentanyl, and metabolites, among the controlled drugs, and nicotine, caffeine, and their metabolites, among the noncontrolled drugs, were studied. Chromatographic separation was achieved in less than 4.5 min, with improved peak resolution and sensitivity. Identification and quantification of the compounds of interest was performed by selected reaction monitoring, using an electrospray ionization source. Isotope dilution (except for paraxanthine) was used for quantitation. Quality parameters of the method were established, and limits of quantification were obtained for controlled drugs in surface waters from 0.1 to 3.1 ng/L and in wastewaters from 0.2 to 4.0 ng/L. Run-to-run and day-to-day precisions were evaluated in different water matrixes (Milli-Q water, surface water, wastewater). To assess the presence of these drugs in real water samples, the optimized method was applied to the analysis of wastewater and surface river water. The analysis of several samples from wastewater treatment plants in northeast Spain revealed the presence of drugs such as cocaine and amphetamine-related compounds, in both influent and effluent samples. Cocaine metabolite and MDMA (ecstasy) were also found in surface waters while nicotine and caffeine were detected in all the analyzed samples. The results obtained demonstrate that the presence of these drugs in the aquatic media must be considered a matter of environmental concern.