A method for the identification and quantification of hydroxyzine in human fluids by GC/NPD is presented. The method employs acepromazine as the internal standard and requires no derivatization. After a single alkaline extraction in n-heptane isoamylalcohol (98.5:1.5, v/v), analysis is achieved in 7 min. The lower limit of detectability was 0.8 ng/ml in plasma. Capillary gas chromatography mass spectrometry assay was developed for confirmation. Toxicological findings, after a fatality involving hydroxyzine are presented as an application of the procedure.