Lipid and protein oxidation in an NADH-Fe enzymic and an ascorbate-Fe nonenzymic system were determined simultaneously. The nonenzymic iron-reducing system gave rapid oxidation of lipid that leveled off at values much lower than those achieved in the enzymic system, which showed a continuous increase over the 1 or 2 h incubation times used. Protein sulfhydryl oxidation was more rapid in the nonenzymic system for total and accessible sulfhydryl groups, but the enzymic system oxidized the inaccessible sulfhydryl groups more rapidly. Both lipid and protein oxidations appeared to begin simultaneously. In the enzymic system, more lipid oxidation was achieved on a molar basis than oxidation of protein sulfhydryl groups, while in the nonenzymic system this was reversed. These data probably reflect the site specificity of the production of oxidizing elements in the two systems. The greater lipid oxidation in the enzymic system suggests that this may be the more important ferric iron-reducing system during storage of fish muscle.