A specific and sensitive high-performance liquid chromatographic method for the quantitative determination of vincamine at therapeutic concentrations in plasma is described. The column was packed with Spherisorb ODS 5 micrometer, and the mobile phase was acetonitrile-potassium phosphate (0.02 M, pH 2.3) (50:50) with a flow-rate of 10 ml/min. Detection was at 230 nm. Using automated large-volume injection of a non-eluting solvent (0.02 M potassium phosphate) the method was capable of the analysis of a large number of samples daily. The coefficient of variation of the procedure was 4.8% at a plasma vincamine concentration of 10 ng/ml