A simple, sensitive and reliable competitive protein binding radioassay using dog transcortin has been developed for the measurement of 11-deoxycorticosterone (DOC) in human plasma. A 1% plasma solution from dexamethasone treated male dogs served as the source of the binding protein. Sephadex LH-20 column chromatography was used for the separation of the steroid prior to assay. The method is sensitive enough to detect 50 pg of DOC. The intra- and interassay co-efficients of variation were 11.5% and 11.3% respectively. Water blanks and plasma blanks from adrenalectomized rats and humans gave negligible readings for DOC. Support for the identity of the steroid being assayed as DOC was obtained by subjecting a plasma pool to multiple radioassays using 4 different binding proteins including 2 anti-DOC antibodies. The values obtained in all 4 systems were in good agreement confirming the fact that DOC was the steroid being measured. Morning plasma DOC levels measured in 29 healthy subjects averaged 8.0 plus or minus 1.2 (S.E.) ng% in 14 males, and 8.7 plus or minus 0.9 (S.E.) ng% in 15 females (p greater than 0.3).