In the present study, surface sediments and sediment cores were collected at the Pearl River Estuary (PRE) and its surrounding coastal area. The samples were analysed for total metal concentrations, metal concentrations in the five operationally defined chemical fractions, and Pb isotopic compositions. The concentrations of Co, Cr, Pb, and Zn of the sediments in the PRE were about twice of those at the adjacent coastal area, while the Cu concentrations of the PRE sediments were four times higher than the sediments at the coastal area. The distribution of Cu, Cr, Pb, and Zn demonstrated a typical diffusion pattern from the land to the direction of the sea. Two hotspots of trace metal contamination were located at the mixed zone between freshwater and marine waters. The distribution of trace metals in sediments showed that the major sources of metal contaminants were probably from the discharges of sewage and other outlets in the west bank of the estuary. The enrichment of metal in the sediments could be attributed to the deposition of the dissolved and particulate trace metals in the water column at the estuarine area. The similar Pb isotopic signatures of the sediments at the PRE and its surrounding coastal area offered strong evidence that the This is the Pre-Published Version.