The water toxicity of the Reconquista river, an urban and industrial polluted watercourse was tested. Surface water samples from two points up and downstream of low and high pollution conditions were assayed. Continuous‐flow renewal bioassays under controlled laboratory conditions were run for 21 days. Alterations in the activity of enzymes involved in ion balance and hepatic metabolism were determined in juvenile carp Cyprinus carpio used as test species. Branchial (Na+K)‐ATPase and hepatic glutamic oxalacetate transaminase (GOT) and glutamic pyruvate transaminase activities were the selected biomarkers of toxicity. Sublethal Cd solutions were used as a reference toxic. Results showed that the activity of the enzymes were affected according to the deterioration of the river water quality. Branchial (Na+K)‐ATPase and liver GOT activity results were reliable indicators to discriminate river water samples of dissimilar pollution state. ©1999 John Wiley & Sons, Inc. Environ Toxicol 14: 313–319, 1999