This chapter is a review of different studies focused on the detection and quantification of contaminants of emerging concern such as human and veterinary pharmaceuticals in aquatic environments from mid-east Argentina (Parana river wetlands), using different analytical techniques. In addition, those environmental screenings have been used to test how tadpoles from native amphibian species (e.g., Rhinella arenarum, Leptodactylus luctator, Physalaemus albonotatus, Trachycephalus typhonius, and Scinax nasicus) respond to observed concentrations of pharmaceutical residues (e.g., diclofenac, dexamethasone, ciprofloxacin, enrofloxacin, dipyrone, and streptomycin) and their metabolites. The summary of different studies demonstrated that the presence of these contaminants in aquatic environments poses a deleterious environmental risk for amphibians.