15.
Development and validation of GC-FID and GC-MS method for
determination of alprazolam in pharmaceutical preparations
Bilal Yilmaza,*and Vedat Akbab
aDepartment of
Analytical Chemistry, Faculty of Pharmacy, Ataturk University,
25240, Erzurum, Turkey
bCriminal Police Laboratory, 25060, Erzurum, Turkey
* Corresponding author: E-mail address:
bilalylmaz@yahoo.com
Tel.:
0442 2311401, fax: 0442 2360962
Abstract:
This
paper describes two rapid, sensitive and specific methods for
determination of alprazolam with internal standard (tetracosane)
in pharmaceutical preparations by gas chromatography (GC) with
flame ionization (FID) and mass spectrometric (MS) detection.
The calibration curves were linear for alprazolam (r2
> 0.99) at the concentration range of 0.25-5 µg mL-1
and 50-1000 ng mL-1 with a limit of quantitation of
200 and 40 ng 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 2.68 and 5.15%,
respectively. The developed GC-FID and GC-MS methods were
applied to a pharmaceutical preparation (Xanax) as tablet form
which do not require any preliminary separation or treatment of
the samples. No interference was found from tablet excipients at
the selected assay conditions. Also, the results obtained from
two chromatographic methods were statistically compared and no
significant difference was found.
Key words: Alprazolam, GC-FID, GC-MS, Validation
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