Abstract: This paper describes two rapid, simple and specific methods for determination of disulfiram with internal standard (medazepam) in pharmaceutical preparations by gas chromatography (GC) with flame ionization (FID) and mass spectrometry (MS) detection. The calibration curves were linear for disulfiram (r > 0.99) at the concentration range of 300-4000 µg mL^-1 and 100-1000 µg mL^-1 for GC-FID and GC-MS, respectively. The relative standard deviation for intra- and inter-day precision was less than or equal to 5.17 and 6.41%, respectively. The developed GC-FID and GC-MS methods were applied to a pharmaceutical preparation (Antabuse) as tablet form which does not require any preliminary separation or treatment of the samples. No interference was found from tablet excipients at the selected assay conditions. The results obtained from two chromatographic methods were statistically compared and no significant difference between methods with respect to mean values and standard deviations at the 95% confidence level. Also, the results were statistically compared with those obtained by the official method using F test.

KEY WORDS: Disulfiram, GC-FID, GC-MS, Validation