VALIDATION OF A GAS CHROMATOGRAPHIC
METHOD FOR METHANOL DETERMINATION
DOINA MOALEŞ1*, ADRIAN FLORIN ŞPAC2, VASILE
DORNEANU3, ELENA BUTNARU1
University of Medicine and Pharmacy “Gr.T.Popa”, Faculty of
Pharmacy, Universităţii Street, 16, Iaşi, România
1Department of Toxicology, Bacău Country Department of Forensic
Medicine Toxicology Laboratory,
2Department of Physical Chemistry,
3Department of Analytical Chemistry
*corresponding author: moldoina@yahoo.com
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Abstract:

In this study we developed and validated a gas chromatographic method for
methanol determination from alcoholic distillates. In order to determine methanol concentrations in alcoholic distillates, an aliquot of samples is analyzed by a gas chromatographic - mass spectrometric (GC-MS) method with an Agilent Technologies 7890 A Chromatograph equipped with a Zebron – Phenomenex, ZB-WAXplus column (60 m x 0.25 mm, 0.25 μm) and Agilent Technologies 5975C inert MSD detector. The temperature program begin from 50°C (constant for 20 minutes), after that, the temperature increase with 10°C/min to 250°C, with He as carrier gas (1 mL/min) and MS detection. The temperature of the source was 230°C and of the quadrupole was 150°C. In these conditions, the method is linear in the 5 – 20000 μg/mL range, the detection limit is 146.4 μg/mL, the quantification limits is 443.5 μg/mL. For precision were obtained the following results: for system precision RSD = 1.0621 %, for method precision RSD = 2.6601 %, for intermediate precision RSD = 2.3336 %. The accuracy was 95.9% in 92.4 – 97.9% range. Under these conditions, methanol was determined from alcoholic distillates with good results.

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