A sensitive gas chromatography/mass spectrometry method for the detection and quantitation of 7-aminoflunitrazepam, the major urinary metabolite of flunitrazepam, is described. The method is based upon solvent extraction followed by derivatisation with methyl-bis-trifluoroacetamide (MBTFA), to give a trifluoroacetyl derivative. A profile of 7-aminoflunitrazepam urinary concentrations following ingestion of 0.5 to 4 mg oral doses is reported. The method has been found to be reproducible and can be used for the confirmation of flunitrazepam administration.