If a great number of rays are fished in the Tropical East Atlantic Ocean for their caudal fins, only a small amount of ray flesh is processed. Among them, three species of rays, Dasyatis marmorata, Rhinobatos cemiculus, and Rhinoptera marginata, from the Mauritanian coast have been investigated for the fatty acid composition of their lipids. Gas chromatography and gas chromatography-mass spectrometry allowed identification of 50 molecules from muscles, livers, and gonads of these fishes. Principal component analysis, starting from >50 samples, reveals significant differences in various fatty acid distributions, related to the species and sex of the sampled fish. Some of them are preferentially present in one sex or in both species, whereas the occurrence of others characterizes the male and female of one or two species. The results show that rays are potential resources of polyunsaturated fatty acids (PUFA) and should be used in the diet of local populations. The lipidic fractions contained a high amount of PUFA (up to 30% of the total), mainly composed of docosa-4,7,10,13,16,19-hexaenoic acid, eicosa-5,8,11,14-tetraenoic acid, and eicosa-5,8,11,14,17-pentaenoic acid.