Polynuclear Aromatic Hydrocarbons (PAHs) were investigated in water and sediment samples from River Benue in Makurdi metropolis. Samples of water and sediment were collected from 6 sites in River Benue during the dry season. The samples were extracted using liquid-liquid extraction and soxhlet extraction methods respectively and analyzed for acenaphthene, fluoranthene, 2-methynaphthalene and naphthalene using gas chromatography coupled to mass spectrometry (GCMS). The results showed that the samples contained very low concentrations of these PAHs (concentrations varied from 0.06 to 8.02 ppb). So, there was little or no threat to fish, wildlife or humans, based on low concentrations determined in the samples but accumulation over time may pose a health risk. Their sources were thought to be natural and anthropogenic, and the varied concentrations at the various points were due to different activities at those points.