Change in the amount of volatile carbonyls (VC) was compared with those of peroxide (PO) and oxidized acid (OA) during storage in mackerel oil and in lipids of cooked fleshes of mackerel and saury-pike. All of the above products increased with the outset of storage. PO, however, reached the maximum at early stage of storage and then declined. OA continued to increase through the whole periods of storage. VC also increased gradually during storage except in prolonged storage of mackerel flesh. Its relative level differed with the difference in the kinds of sample (Figs. 1-4). Then, VC may be used to follow the development of rancidity in a given fatty material. Admixture of antioxidants to fish inhibited VC formation. Inhibitory effect was pronounced with BHA (tech.),PG(tech.) and NDGA. Ascorbate also exserted some inhibitory effect, though it accelerated the discoloration of flesh (Fig. 5). Against VC formation, most of amino acids tested were inhibitory, while ferric and cupric ions in smaller amount acceleratory (Figs. 6 and 7).