In the present work, a simple method of sample preparation for the determination of polycyclic aromatic hydrocarbons (PAHs) in water rich in colloidal particulate was developed. The technique was mainly based on the effect of the flocculation of aluminum sulfate and the adsorption of the flocculation aid florisil. The method contained three steps: flocculation, ultrasonic extraction, and solid-phase extraction cleanup. Major parameters of the procedure were optimized with high performance liquid chromatography (HPLC) separation and ultraviolet-fluorescence detection. When 250 mL model sample containing 16 EPA PAHs was processed, the developed method provided detection limits in the range of 0.02-5 ng/L. Both spiked and non-spiked polluted river water samples rich in suspended particles and organic matters were analyzed. Recoveries and relative standard deviations for the 16 PAHs were in ranges of 86-94% and 3-13% (n = 5), respectively.