A simple method of extraction and determination of sixteen priority polycyclic aromatic hydrocarbons (PAHs) from waste water and sediment using high performance liquid chromatography (HPLC) has been validated with limits of detection (LOD) and limits of quantification (LOQ), method recovery and reproducibility and other factors. HPLC parameters, such as mobile phase composition and flow standardized for determination of PAHs using ultra violetdiode array detector (UV-DAD). PAH extraction was carried out by liquid-liquid and Ultrasonication using dichloromethane and acetone/hexane solvents for water and sediment, respectively. Silica gel column chromatography was carried out for extract clean-up. Linearity of calibration curves was good for all sixteen PAH (R2, 0.991-0.996) in the concentration range 2.5-300 ppb. Analysis of standard spiked water and sediment samples resulted in good recoveries between 78-100% and 82-106%, respectively. The estimated LOD and LOQ ranged between 0.01-0.51 ppb and 0.03-1.71 ppb, respectively. The method described has been used for determination of the sixteen PAHs contents in water and sediment samples collected from municipal drains.