12.
Development and Validation of GC-FID and GC-MS Method for
Determination of Disulfiram in Pharmaceutical
Preparations
Bilal
Yilmaza,* and Meltem Cetinb
aDepartment of Analytical Chemistry, Faculty of Pharmacy, Ataturk
University, 25240, Erzurum, Turkey
bDepartment of Pharmaceutical Technology,
Faculty of
Pharmacy, Ataturk University, 25240, Erzurum, Turkey
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
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