The main objective of this study was to evaluate the metal content in water and sediment from the Toledo municipal lake, as well as the concentration levels of heavy metals in muscle and liver of four fish species. A digestion procedure was performed in all fish samples. Metal analysis was performed by using the Synchrotron Radiation X-ray Fluorescence technique. The accuracy and validity of the measurements were determined by analysis of certified reference materials. The highest Cr, Cu and Se concentration levels above the maximum tolerance limit according to the Brazilian norms in fish tissue could be associated with the metal uptake and accumulation due to the direct contact with contaminated water and sediment. © IWA Publishing 2011.