A method for the simultaneous extraction and HPLC analysis of nitrophenols and poly-aromatic hydrocarbons (PAHs) in aquatic samples is presented. The efficiency of the solvent extraction and the solid phase extraction (SPE) is compared. The results showed that the polymeric SPE sorbent is the best compromise for the simultaneous extraction of the tested compounds taking into consideration the lipophilicity of PAHs and the polarity of nitrophenols. The best results were obtained on polymeric Strata X sorbent, elution with dichloromethane followed by elution with methanol. Silica gel C18 sorbent is improper for nitrophenols due to the strong interactions with the residual hydroxyl groups of silica gel. The developed SPE-HPLC method was successfully applied for the analysis of these pollutants in different water samples.