A sensitive and specific HPLC method has been developed for the assay of vigabatrin in human plasma and urine. The assay involves derivatization with 4-chloro-7-nitrobenzofurazan, solid-phase extraction on a silica column and isocratic reversed-phase chromatography with fluorescence detection. Aspartam. was used as an internal standard. The assay was linear over the concentration range of 0.2-20.0 mug/ml for plasma and 1.0-15.0 mug/ml for urine with a lower limit of detection of 0.1 mug/ml using 0.1 ml of starting volume of the sample. Both the within-day and day-to-day reproducibilities and accuracies were less than 5.46% and 1.6%, respectively. After a single oral dose of 500 mg of vigabatrin, the plasma concentration and the cumulative urinary excretion of the drug were determined. (C) 2001 Elsevier Science B.V. All rights reserved.