1. Eight young healthy persons, four men and four women, were maintained for a total of 2 months on a diet in which 40%, 16% and 44% of the total calories were present as fats, proteins and carbohydrates respectively. The ratio of complex to simple carbohydrates in the diet was 1:4. 2. The fatty acids of serum kephalins, lecithins, lysolecithins and sphingomyelins were determined by gas–liquid column chromatography. 3. Lysolecithins in both men and women had the highest content of saturated acids, followed by sphingomyelins, lecithins and kephalins in that order. The degrees of saturation and of polyunsaturation of the fatty acids in the different phospholipid fractions were significantly different, except for the differences in the polyunsaturation of the kephalins and lecithins. 4. No sex difference was found in the fatty acid composition of the different phospholipids.