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Aquaculture wetlands, particularly those located within urban areas, are fragile ecosystems due to urban and aquaculture impacts. However, to date, there are no reports on the combined toxicity of heavy metal mixtures in aquatic biota in sediments from aquaculture wetlands in metropolitan areas. Thus, the characterization, bioavailability, and ecological probability risk of heavy metals were studied in the riverine/estuarine sediments of the Rongjiang River in an aquaculture wetland in Chaoshan metropolis, South China. In the study area, the average total concentrations (mg/kg) were 2.38 (Cd), 113.40 (Pb), 88.27 (Cr), 148.25 (Ni), 62.08 (Cu), 125.18 (Zn), 45,636.44 (Fe), and 797.18 (Mn), with the Cd pollution being regarded as extremely serious based on the enrichment factor (EF). There are two main sources of heavy metals in the study area; Ni, Pb, Zn, Fe and Mn are mainly from domestic waste, while Cr, Cd and Cu are possibly associated with industrial production activities. The bioavailability of most heavy metals accounted for more than 20% of the total concentration. The combined toxicity of heavy metal mixtures based on probabilistic risk assessment suggests that the surface sediments of the Rongjiang River and its estuary had a 15.71% probability of toxic effects on aquatic biota. [Display omitted] • MetaLs in sediments from a metropolitan aquaculture wetland were investigated. • Cd pollution was extremely serious based on enrichment factor (EF) method. • Most metals contributed over 20% of bioavailable concentration to their total. • Surface sediments had a 15.7% probability of toxic effects on aquatic biota. [ABSTRACT FROM AUTHOR]