A quantitative assessment of pollutants of emerging concern in the Hartbeespoort Damcatchment area was conducted using liquid chromatography-tandem mass spectrometry LC-MS/MS) to establish the occurrence, source and distribution of 15 environmental pollutants, including 10 pharmaceuticals, 1 pesticide and 4 steroid hormones. Seasonal sampling was conducted in the Hartbeespoort Lake using sub-surface grab sampling to determine the lake's ecological status and obtain data for establishment of progressive operational monitoring. The Jukskei River, which lies upstream of the Hartbeespoort Dam, was sampled in the winter season. Five year old carp Cyprinus carpio) and catfish Clarias gariepinus) were also sampled from the Hartbeespoort Dam to study bioaccumulation in biota as well as to estimate risk associated with fish consumption. In the Jukskei River, the main source of 11 emerging pollutants EPs) was identified as raw sewage overflow, with the highest Sigma 11 EP concentration of 593 ng L-1 being recorded at the Midrand point and the lowest Sigma 11 EP concentration of 164 ng L-1 at the N14 site located 1 km downstream of a large wastewater treatment plant. The Jukskei River was found to be the largest contributor of the emerging contaminants detected in the Hartbeespoort Dam. In the Hartbeespoort Dam EP concentrations were generally in the order efavirenz > nevirapine > carbamazepine > methocarbamol > bromacil > venlafaxine. Water and sediment were sampled from the uMngeni River estuary within 24 h after large volumes of an assortment of pharmaceuticalwaste had been discovered to bewashed into the river estuary after flash rainfall on 18 May 2016. Analytical results revealed high levels of some emerging pollutants in sediment samples, up to 81 ng g(-1) for nevirapine and 4 ng g(-1) for etilefrine HCL. This study shows that efavirenz, nevirapine, carbamazepine, methocarbamol, bromacil and venlafaxine are contaminants that require operational monitoring in South African urban waters.