The Barigui River watershed is located in the metropolitan region of Curitiba, southern Brazil, passing through several neighboring counties. In recent years, due to growth and disorderly occupation along the river, in addition to lack of sanitation, the Basin suffered a very large inflow of untreated domestic sewage. Current programs to monitor the watershed use traditional physical-chemical parameters and generally the analysis is performed only with water samples. This study analyzes the presence of fecal sterols in sediment samples. Sediment samples were collected from six points along the river and the stanols were extracted, purified and analyzed by GC-MS. Eight compounds were analyzed, among sterols and ketones. The presence of coprostanol was also identified. Coprostanol is a stanol containing a large amount in human feces. It is found near sources of pollution and can be associated with contamination by domestic sewage. The results showed high concentrations of coprostanol, ranging from 0.25 to 196 mug g( - 1). The ratio of coprostanol and epicoprostanol, was below 0.20 at most stations, indicating that the sewage discharged into the river does not undergo prior treatment. Contamination by untreated sewage was also confirmed by ratios of isomeric forms of sterols and ketones 5beta/(5beta + 5alpha).