The study determined the types of pesticide/herbicide pollutants in water, sediment and fish from the Kafue River. A preliminary investigation of the oxidative stress from these pesticides/herbicides was also assessed by measurement of catalase activity. Water, sediment and fish samples were collected upstream, midstream and downstream the Kafue river in Chingola, Kitwe, Kafue National Park and Kafue Town. Water, sediment and fish muscle were sampled and analysed for pesticides using Gas chromatography. For catalase activity fish liver samples only were examined. The pesticides/herbicides detected in all samples collectively included: Heptachlor, pp'-DDE, Cypermethrin, Chlordane, Toxaphene, Terbufos, Kelthane, Endosulfan, Dieldrin, pp'-DDD, pp'-DDT, Atrazine, Disulfoton, d-trans-Allethrin and Endrin. On the other hand, catalase activity was detected in all fish liver samples from all sites. Its levels increased significantly from Chingola upstream to sites down-stream with highest being in Kafue town. This study therefore, demonstrates that there is widespread contamination of the Kafue River with pesticides/herbicides. It also demonstrates that organochlorides are found throughout the river especially in fish samples. The spectrum of pesticides/herbicides was much wider in fish probably due to bioaccumulation. It was also observed that fish are subjected to oxidative stress as determined by catalase levels. The stress is more pronounced downstream where the catalase levels were significantly higher than Chingola. The observation that more pesticide varieties are also found downstream may suggest a likely causative effect of the pesticides on oxidative stress although this needs further investigation. This study further tentatively highlights the potential dangers of these agro-related substances to dependants of the Kafue River water body and the need to carry out risk assessments and thereafter institute corrective measures to help reduce contamination and adverse effects.