Vasopressin levels and vasopressin-converting aminopeptidase activity were measured in the rat pineal gland during the 24 hr light-dark cycle. A rhythmic variation in peptide levels and peptidase activity occurred. At the onset of light at 6.00 hr, the peptidase displayed a significant, short-lasting (approximately 3 hr) increase of about 35% in activity, while a decrease of 28% in pineal vasopressin levels was observed. The changes in peptidase activity and peptide level were not triggered by light per se, since they persisted to occur at the same time point in animals which were not exposed to light, indicating the circadian nature of the rhythmicity. These changes were specific to the pineal gland, since other tissues, like hippocampus and pituitary gland, did not show these daily variations. The data suggest a relationship between vasopressin levels and vasopressin-converting aminopeptidase activity.