Pharmaceuticals and illicit drugs are contaminants that are generally ubiquitous in wastewater treatment plant effluents with their release into the environment being well understood in North America, Europe, and Asia. There is, however, less information on the release of human pharmaceuticals and illicit drugs from regions undergoing rapid land use, economical, and social changes, such as Brazil. This encompasses many areas in the tropical zone where releases of emerging contaminants may impact pristine, bio-diversity rich ecosystems. In this study, the occurrence of human pharmaceuticals and the illicit drug cocaine was determined in the Rio Negro and two of its tributaries that receive large amounts of untreated sewage, the Igarap e Mindu and the Igarap e do 40, passing through the city of Manaus, Brazil. In addition to cocaine and its metabolite, benzoylecognine, propranolol, diclofenac, amitriptyline, carbamazepine, carbamazepine-epoxide, citalopram, metoprolol, carisoprolol, and sertraline were all detected in two urban tributaries at low ng/l concentrations similar to those typically found in urban surface waters. Concentrations in the Rio Negro were typically lower than detection limits due to the large level of dilution, although traces of a range of pharmaceuticals were detected in the Rio Negro in proximity of the confluence of the urban streams. The data represent new information on the emissions of pharmaceuticals from a newly industrialized region of Brazil.