A method was developed to assay α-Hydroxyltriazolam and α-Hydroxyalprazolam,　which are the major metabolites of triazolam and alprazolam respectively,in human urine.　After addition of 2-hydroxyflurazepam　(interal standard) and hydrolysis with β-glucuronidase, the hydroxy-metabolites were extracted with hexane-dichloromethane (1∶1) at pH　10.8, then were derivated with (BSTFA). The analysis was performed on a HP-5 capillary column with electron-capture detector.The detection limits of analysis in urine were about 1μg/L.The method was successfully applied to urine specimens collected from healthy human volunteers who ingested 0.5 mg of triazolam or 0.8 mg alprazolam. The method was enough sensitive to assay urine specimen excreted at 24 h by volunteers after taking the medicine.