Synaptosomes from sheep brain cortex were incubated with carrier-free Na235SO4 and the synaptic plasma membranes were isolated. The membranes were free of contamination from cytosol, mitochondria and microsomal material and accounted for 30% of the radioactivity present in the synaptosomal particulate fraction. Control experiments demonstrated that the radioactivity present in the preparation was not due to non-specific binding of sulphate ions. The synaptic membranes contained at least six 35S-containing protein bands with molecular weights between 160 000 and 16 000. Analysis showed that the radioactivity was located in the carbohydrate moiety of a glycopeptide.