THE PROCESS AND VALIDATION OF METHANOL DETERMINATION FROM BIOLOGICAL SAMPLES BY MEANS OF A GAS-CHROMATOGRAPHIC METHOD TOGETHER WITH MASS SPECTROMETRY
Doina Moales(1), Adrian Florin Spac(1), Maria Prisecaru(2), Elena Butnaru(1)
1. University of Medicine and Pharmacy “Gr.T.Popa”, Faculty of
Pharmacy, Universitatii street, no. 16, Iasi, Romania, Department of Toxicology, Department of Physical Chemistry e-mail: moldoina@yahoo.com
2. „Vasile Alecsandri” University of Bacau, Faculty of Science, Department of Biology, Marasesti Street, no. 157, Bacau, Romania e-mail: prisecaru_maria@yahoo.com
Abstract
In order to determine the methanol
concentration, the biological samples (blood,
tissues) were analyzed by an Agilent
Technologies 7890 gas chromatograph with an
Agilent Technologies 7683 Series automatic
injector equipped with a Zebron – Phenomenex,
ZB-WAX plus column (60 m x 0.25 mm, 0.25
µm), and Agilent Technologies 5975C inert MSD
detector; data acquisition was made by SIM
method. Data interpretation: Agilent
Technologies ChemStation software. The
temperature program begins from 50°C (constant
for 16 minutes), after that. the temperature
increase with 25°C/min up to 250°C, the mobile
phase (He) with a debit of 1 ml/min. The source
temperature is 230°C and the quadruple’s is 150
°C. In these conditions. the method is linear in the
5 – 20000 μg/mL range. the detection limit is
417.8 μg/mL, the quantification limits is 1266.1
μg/mL. There were determined: the system’s
precision (RSD = 0.8748%), method precision
(RSD = 4.6811%), intermediate precision (RSD =
4.1078 %); the accuracy was 98.0% in 93.2 –
102.8% range. Under these conditions, the
methanol concentration was determined from
biological samples, that is, blood and tissues.