A simple, sensitive and selective method for the determination of ximoprofen and its keto and hydroxy metabolites in human urine has been developed using high-performance liquid chromatography in the reversed-phase mode. The limit of reliable determination of ximoprofen and each of its metabolites in urine is about 1 microgram/ml (4 nmol/ml). The method has been applied to urine samples obtained from human volunteers after administration of single intravenous doses of 30 mg of ximoprofen and about 70% dose was accounted for in terms of these compounds and their glucuronic acid conjugates.