This study was undertaken to determine the possibility of potential impact of PAHs on the aquatic biota. First, we had developed a new method for measuring 13 different priority pollutant PAHs in waste water samples. Then, eight different water samples collected from different sites along the Menderes River were analysed by this method involving SPE extraction and reverse-phase HPLC. The method presented here is suitable for rapid and accurate determination of PAH in surface waters and the PAH recoveries are practically quantitative. The levels of PAH in the analyzed samples range from 1.8 mu g/L to 24.9 mu g/L and industrialized areas were found to be highly polluted.