Polycyclic aromatic hydrocarbons (PAHs) are measured in surface sediments from rivers and estuary of Pearl River Delta and its nearby South China Sea. Total PAH concentration varied from 255.9 - 16 670.3 ng/g and a moderate to low level compare to relevant areas worldwide. The order of PAHs concentration in sediments was: rivers of Pearl River Delta > estuary > South China Sea, and the most significant PAH contamination was at Guangzhou channel of Zhujiang river. A decrease trend for PAHs concentration with distance from estuary to open sea can be sees in South China Sea. Coal and biomass combustion is the major source of PAHs in nearshore of South China Sea, and petroleum combustion is the main source of pyrolytic PAHs in rivers and estuary of Pearl River Delta according to PAHs diagnostic ratios. Petroleum PAHs are revealed have a high contribution to PAHs in Xijiang River, estuary and some stations in Zhujiang River. A comparison of data from study in 1997 with data from present study indicates that there is no clear change in the PAH concentration over time but the source of PAHs in Pearl River Delta have been change from a main coal combustion to petroleum combustion and being reflect in the sediments in rivers and estuary of Pearl River Delta where there have high sedimentation rate.