Chlorodesmethyldiazepam (I) concentrations were followed for 72 h in the plasma of four volunteers given 2 mg of the drug orally. The drug appears to be well absorbed, reaching peak plasma levels of 20--30 ng ml-1 1--2 h after administration; 72 h after administration, plasma concentrations are still measurable (5 ng ml-1). The analytical method involved a single extraction of I from the plasma into benzene followed by centrifugation, evaporation, and gas-chromatographic analysis of the samples.