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This paper describes a simple, sensitive and rapid method for the determination of triclosan and ketoprofen in wastewater influent, effluent and river water. The method involves solid phase extraction (SPE) of target compounds using Oasis HLB sorbent. Several extraction parameters such as sample pH, sample volume, SPE cartridge and SPE elution solvent were optimized. The pH of the collected samples was adjusted to 5.5, and then 100 mL of the sample was loaded into an Oasis HLB cartridge. Methanol was used to elute the retained compounds. The eluted compounds were analyzed using reversed-phase high performance liquid chromatography with photo diode array detection (HPLC-PDA). The method was validated by spiking ultra-pure water and wastewater with different concentrations of both compounds ranging from 5 mu g L-1 to 1000 mu g L-1. Recoveries were in the range of 73% to 104 %, and% RSD ranged from8% to 15%. The method gave good detection limits of 0.01 and 0.08 mu g L-1 for triclosan and ketoprofen, respectively. Traces of both compounds were detected in all wastewater (influent and effluent) samples at a range of 1.2 to 9.0 mu g L-1 and in some river water samples.