The generally accepted methods for the synthesis of triglycerides are unsatisfactory when they are applied to highly unsaturated systems such as those present in fish oil. The methods either fail to g ive sufficiently high yields, or they are prohibitive in cost when applied to large scale production. Of the numerous reactions studied, the most feasible was the zinc‐catalyzed esterification of fish oil fatty acids with glycerol. Thinlayer chromatography (TLC) showed that this reaction gave yields of 75舑78% triglycerides. Gas‐liquid chromatography (GLC) demonstrated the composition of the triglycerides was essentially the same as that of the original fatty acids.