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A radioimmunoassay for oxytocin in aqueous solution is described, with a sensitivity comparable with the best current bioassays. It is highly specific; arginine-vasopressin and lysine-vasopressin interfere only at 1000-fold greater concentration, while bradykinin, histamine, acetycholine and many other substances, which interfere with some bioassays, have no effect. In certain circumstances, there is a dissociation between loss of biological and immunological activity. Thus reducing agents had no effect on immunological activity, in contrast to their effect on biological activity. In late pregnancy plasma, the biological activity of oxytocin is destroyed more rapidly than the immunological activity. Radioimmunoassays have considerable advantages over bioassays both in convenience and specificity. However, bioassays should be employed for reference purposes because of the dissociation between biological and immunological activity that may occur.