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Polycyclic aromatic hydrocarbons (PAHs) are major organic pollutants in the environment, which are toxic to humans and biota, given their carcinogenic, mutagenic and teratogenic nature. In this chapter, we carried out an overview of the sources and toxicity of PAHs, their common analytical methods of determination in the water and sediment samples, and also their global trend of distribution, with a view to provide baseline guidance for relevant control authorities. The choice methods for determining these contaminants are high-performance liquid chromatography (HPLC) with UV/fluorescence detectors and GC/MS. Mass spectrometer coupled with GC is preferred because it offers robust identification of the analyte compounds both by retention time and mass spectrum, with additional structural information. Results collated revealed an extensive distribution of PAHs with total mean concentrations ranging from 0.0003 to 42,350 μg/L in water and 0 to 1.266× 109 μg/kg (dw) in the sediment. PAHs in the two environmental matrices were much higher in the regions with intense oil exploration, shipping and industrial activities. It is therefore necessary to regularly monitor their levels in the aquatic environment, so as to provide mitigation options that will prevent risk to humans and aquatic animals.