A sensitive and simple HPLC method with fluorimetric detection has been developed for determination of droperidol in pharmaceutical tablets, human serum, and human milk. Chromatography was performed on a 100 mm x 3 mm i.d. C-18 column with methanol-water, 30:70 (v/v), PH 3.5, as mobile phase at a flow-rate of 0.8 mL min(-1). The injection volume was 5 mu l. and detection was by monitoring emission at 324 nm after excitation at 283 nm. Droperidol and p-hydroxybenzoic acid (internal standard) eluted after 5.3 and 6.1 min, respectively. The method was validated over the concentration range 1.14 X 10(-7) to 9.12 x 10(-6) M. Selectivity was good and the limits of detection and quantitation of the method were approximately 3.54 x 10(-8) and 1.07 x 10(-7) M, respectively, corresponding to 13 and 40 ng mL(-1). The applicability of the method to determination of droperidol in pharmaceuticals, human serum, and human milk was demonstrated.