Freshwater fish Oreochromis niloticus were exposed to 5, 10 and 20 microM concentrations of Cd, Cu, Zn and Pb for 14 days and responses of several enzymes were determined subsequently. Liver catalase (CAT) activity was influenced by Cd and Pb exposures, while it was inhibited by Zn exposure. Copper, on the other hand, did not cause significant changes in CAT activity. Liver alkaline phosphatase (AP) activity was first stimulated at lowest (5 microM) exposure concentration, while there were significant inhibitions at higher (10 microM) exposure concentration. At the highest (20 microM) exposure concentration, AP activity was compensated coming to the control level, except Pb exposure. Intestine and serum AP activities were stimulated by all Zn exposures and 10 microM Cu exposure, while other exposures did not cause significant changes on AP activity. Na,K-ATPase activity in the gill and intestine was inhibited by all the metal exposures, except 20 microM Pb exposure that resulted in an increase in the activity in the gill. Similarly, muscle Ca-ATPase activity was inhibited by all the metal exposures, except Cu exposures. This study indicated that enzymatic systems may be used as a sensitive bioindicator of metal contamination in aquatic systems. Nevertheless, the results also stress the importance of addressing the sensitivity of these enzymes when they are used as a bioindicator for metal contamination, because the responses of the enzymes varied considerably according to metal types and concentrations.