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Wastewaters are considered one of the main sources of pollution in the aquatic environment as release a large number of contaminants every day. Emerging contaminants such as pharmaceuticals have special interest due to the high levels of consumption by the global population, their bioactive properties and because actual directives do not include the monitoring of pharmaceuticals. Moreover, it is well-known that pharmaceuticals can be degraded to metabolites or transformation products (TPs), which could be more toxic than the parental compound. In this study, we have developed an analytical method based on solid-phase extraction (SPE) and liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) to determine 76 highly consumed pharmaceuticals, including metabolites and TPs in wastewater effluents. In the 10 wastewaters analysed, the mean concentrations were in the µg L−1 levels, being mycophenolic acid, levodopa, ibuprofen, 4-aminoantypirine, losartan, amylmetacresol, amoxicillin, fluticasone, tramadol, budesonide, chlorpheniramine and diclofenac the pharmaceuticals with the highest concentrations. This study provides a comprehensive optimization on the MS conditions to determine pharmaceutical compounds and their metabolites and provides a spectral characterization to be used for the identification of these compounds in water.