A simple, rapid, and sensitive method for determining 10 arylamine compounds in wastewater sample using solid-phase extraction (SPE) and high performance liquid chromatography (HPLC) with UV detection is developed. An SPE procedure is described for extracting and preconcentrating the arylamines on Sep-Pak C18 cartridges with methanol as solvent. A mobile phase gradient of acetonitrile-water was used for the separation and determination of the arylamines.