In this study, an evaluation of suitable extraction and clean up techniques for benzophenones of gidazepam in urine samples was done. Solvent extraction methods were compared with solid-phase extraction using Bond Elut Certify. For end-step detection method two–dimensional gas chromatography-mass spectrometry (GC-GC/MS) were evaluated. Presence of aminocarboxibromobenzophenone in the urine was an indicator of the subject being a probable abuser of gidazepam.