After the Aznalcóllar mining spill (April, 1998) different ecosystems along the Guadiamar river and the Guadalquivir estuary were impacted by high concentrations of metals. The concentration of metals Zn, Cd, Pb, Cu and As has been detected as a good tracer of the pathway of the toxic spill. Different individuals of the fish Solea senegalensis and the clam Scrobicularia plana were exposed to contaminated sediments after the accidental spill in the south-west Spain. The induction of metallothioneins in fish and the bioaccumulation of metals in clams were determined in different tissues to determine the biological adverse effect associated with the heavy metals from the spill. A relationship between the enrichment of metals in the tissues and the induction of metallothioneins was determined for those assays performed using contaminated sediments. The bioaccumulation of metals indicates that the risk associated with the spill should be continuously evaluated to establish the sublethal effects related to the accident.