A field study in the Pearl River Delta of China was conducted in order to describe to the spatial and seasonal variation of occurrence and concentrations of total petroleum hydrocarbon (TPH) in surface water and sediments. Petroleum hydrocarbons and isoprenoid alkanes were quantified by UV spectroscopy and gas chromatography with a mass selective detector. The concentrations of TPH ranged from 4.3 to 68.7 µg L−1 in surface water, and from 66.6 to 1445 µg g−1 in surface sediments. The ratios of pristine to phytane suggested that the main sources of TPH in the sediment were petroleum importation. The highest concentrations of TPH were present in the spring season. When compared with results from previous studies, it can be concluded that the Pearl River Delta was moderately polluted by TPH. No statistically significant correlations were observed between the concentrations of TPH in surface water and sediments.