A rapid, precise, accurate, and selective high-performance liquid chromatographic method with fluorescence detection has been validated and used for analysis of amisulpride in human plasma after a simple solid-phase extraction procedure. Compounds were separated on a CN column with 0.03 M potassium dihydrogen phosphate (pH 6.5)-acetonitrile 65:35 (v/v) as mobile phase. Fluorescence detection was performed at excitation and emission wavelengths of 274 and 370 nm, respectively. Calibration plots were linear over the concentration range 10-1,000 ng mL(-1) in human plasma, and the lower limit of quantification was 10 ng mL(-1). Accuracy was between 0.4 and 6.4% and precision was between 3.1 and 7.5%. Amisulpride was sufficiently stable through three freeze-thaw cycles, during storage for 6 h at room temperature, and for 2 months at -22 °C. The method is suitable for the analysis of clinical samples from pharmacokinetic studies.