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Polycyclic aromatic compounds continue to be regarded as a major environmental threat, especially in the aquatic environment. To gather further information on the distribution and levels of these persistent organic compound in natural waters, the current analytical study was carried out. Material collected from multiple sites within the coastal and open sea areas of several surface water bodies had different levels of polycyclic aromatic compounds. Concentrations of dissolved, particle- and biota-associated compounds (i.e., benzo (a)pyrene, benzo(e)pyrene, pyrene, chrysene and so on) were measured by multiple analytical techniques. The sediment and biota samples were extracted using Soxhlet extraction followed by analysis using reverse-phased liquid chromatography with ultraviolet and fluorescence detection and high resolution luminescence spectroscopy. This group of pollutants was significantly enriched in particulate matter, sediments and biota material at all sites relative to water concentrations. On the basis of data obtained, the enrichment factors of 10 to 105 for different carcinogenic and noncarcinogenic compounds in the particulate material and biota are reported. Higher concentrations of the more hydrophobic compounds were found in sediments. Thus, the bottom biota may be exposed to higher levels of hydrophobic pollutants than organisms residing in the upper sediment-water interface.