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Although heavy metal pollution has developed into a major global environmental problem, most research has focused on specific elements, especially arsenic (As) and selenium (Se), and on the health risks to people in polluted areas or by occupation. This study investigated the urine of 480 participants from Guangzhou with a population of 18 million and targeted nine heavy metals: As, Se, chromium (Cr), manganese (Mn), nickel (Ni), cadmium (Cd), lead (Pb), antimony (Sb), and mercury (Hg). The heavy metals were widely detected, of which As, Se, Cd, and Pb all exceed 98%. Among the toxicants, As showed the highest concentration, followed by Se with 40.5 and 35.4 μg/L, respectively. The heavy metal levels from suburban subjects were generally higher than those in urban subjects (except for Sb), and the Cd level of males was lower than that of females. Concentrations were related to age, body mass index, alcohol consumption, and smoking. According to the health risk assessment, most subjects experienced potential non-carcinogenic risk from As, Cd, Se, and Hg, which accounted for 38.2%, 8.83%, 8.31%, and 3.38%, respectively. The carcinogenic risk of As and Cd surpassed the risk level of 10−6, and 90.1% and 35.4% of the subjects, respectively, exceeded 10−4, an unacceptable risk level. More attention to the high carcinogenic risk from heavy metals and the high detected levels of As and Cd is required.

“Swimming across the Pearl River” is an annual large-scale sporting event with great popularity in Guangzhou. To reduce the risk of swimmers’ exposure to various contaminants in the Pearl River during swimming activities, the local government limits direct sewage and effluent discharge from urban channels during the event. However, the impact of discharge reduction on some contaminants of emerging concern (CECs), such as organophosphorus flame retardants (OPFRs), bisphenol analogues (BPs), and triclosan remains unknown. In the present study, the concentrations of CECs, as well as ammonia-nitrogen (NH3-N), dissolved organic carbon, and chemical oxygen demand, were measured in aqueous and suspended particulate matter (SPM) from the Guangzhou reaches of the Pearl River. The concentration ranges of sixteen OPFRs, eight BPs, and triclosan were 21.2–91.0, 8.46–37.3, and 1.47–5.62 ng/L, respectively, in aqueous samples, and 25.2–492, 14.0–86.3, and 0.69–17.5 ng/g, respectively, in SPM samples. Hydrophobic and π-π interactions could be contributing to the distribution of CECs. Principal component analysis indicated that consumer materials, manufacturing, and domestic sewage might be the main sources of the CECs. In addition, our study showed that the concentrations of CECs did not change considerably before or after discharge reduction activities, although NH3-N showed a substantial decrease following pollution control measure. The results demonstrated that temporary reductions of contaminant discharges to the Pearl River had only limited effect on the levels of CECs. Further research is needed to investigate the distributions and potential health risks of CECs in the Pearl River.