We developed a simple method to determine benzodiazepines in biological samples using electron capature detectors and nitrogen-phosphorous detectors. The extraction of 13 benezodiazepines in urine at pH 9.5 with toluene and its analysis in GC/NPD showed the peaks in 9-16 min. In this retention time range, the biological backaground was fairly low and the drugs could be identified in low concentrations. The benzodiazepines in urine samples were screened by the fluorescence polarization immunoassay and positive samples were confirmed by the GC/NPD method.