A highly sensitive and selective glass capillary gas chromatographic negative ion chemical ionization mass spectrometric assay was developed to measure peptidoaminobenzophenone(2-o-chlorobenzoyl-4-chloro-N-methyl-N'-glycylglycinanilide) and its metabolites; chlorodiazepam, chlorodesmethyldiazepam and lorazepam in human plasma. As peptidoaminobenzophenone underwent pyrolysis during gas chromatography, it was converted to a thermally stable aminoquinolone. Internal standards for these compounds were the respective deuterium labelled compounds. Calibration curves were prepared for the range of 1-100 ng ml-1. Interference by endogenous substances was negligible in the isobutane negative ion chemical ionization mode in contrast to the electron impact or positive ion chemical ionization mode. This method was used to determine the plasma levels in humans following oral administration of two 5 mg doses.