The major phosphoglycerides from ox brain myelin and mouse brain microsomal, mitochondrial and myelin fractions were separated by preparative thin layer chromatography. Alk-l-enyl groups from the alk-1 -enyl acyl gly c er o p hosphorylethanolamines were reacted with 1,3-propanediol to form the 1,3-dioxolane derivatives. Acyl groups were converted to the methyl ester derivatives and the acyl groups from alk-1enyl acyl glycerophosphorylethanolamines and diacyl glycerophosphorylethanolamines were also determined separately. The acyl and alk-l-enyl group compositions of the phosphoglycerides from microsomal and mitochondrial fractions were quite similar. The ethanolamine and serine phosphoglycerides contained large amounts of 18:0, 18:1, 20:4 and 22:6 acyl groups. The choline phosphoglycerides had small amounts of polyunsaturated acyl groups and large amounts of 16:0, 18:1 and 18:0 acyl groups. The mitochondrial cardiolipins contained unusual amounts of several acyl groups including 18: 1, 52%; 18:2, 6%; and 16.1, 4%. A large portion of the mouse brain 18:2 is in that fraction. The myelin phosphoglycerides were deficient in saturated and 22:6 groups and markedly enriched in 18:1 and 20" 1 groups when compared with the corresponding microsomal or mitochondrial phosphoglycerides.