Samples of treated effluent and treated and untreated water were collected at 20 municipal wastewater and drinking-water treatment facilities in the Tar and Cape Fear River basins of North Carolina during 2003 and 2005. The samples were analyzed for a variety of prescription and nonprescription pharmaceutical compounds and a suite of organic compounds considered indicative of wastewater. Concentrations of these compounds generally were less than or near the detection limits of the analytical methods used during this investigation.