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  • Simultaneous Determination of Methanol, Ethanol and Formic Acid in Serum and Urine by Headspace GC-FID.

Simultaneous Determination of Methanol, Ethanol and Formic Acid in Serum and Urine by Headspace GC-FID.

Journal of analytical toxicology (2015-07-17)
Miroslava Bursová, Tomáš Hložek, Radomír Čabala
ABSTRACT

A simple, cost-effective headspace gas chromatography (GC) method coupled with GC with flame ionization detection for simultaneous determination of methanol, ethanol and formic acid was developed and validated for clinical and toxicological purposes. Formic acid was derivatized with an excess of isopropanol under acidic conditions to its volatile isopropyl ester while methanol and ethanol remained unchanged. The entire sample preparation procedure is complete within 6 min. The design of the experiment (the face-centered central composite design) was used for finding the optimal conditions for derivatization, headspace sampling and chromatographic separation. The calibration dependences of the method were quadratic in the range from 50 to 5,000 mg/L, with adequate accuracy (89.0-114.4%) and precision (<12%) in the serum. The new method was successfully used for determination of selected analytes in serum samples of intoxicated patients from among those affected by massive methanol poisonings in the Czech Republic in 2012.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
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Ethanol Fixative 80% v/v, suitable for fixing solution (blood films)
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Ethanol standards 10% (v/v), 10 % (v/v) in H2O, analytical standard
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N,N′-Bis(acryloyl)cystamine, BioReagent, suitable for electrophoresis
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Isopropyl alcohol, ≥99.7%, FCC, FG
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3-Methyl-2-pentanone, 99%
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Sulfuric acid, 99.999%
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Sulfuric acid, ACS reagent, 95.0-98.0%
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Methanol, ACS reagent, ≥99.8%
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Sulfuric acid, puriss. p.a., for determination of Hg, ACS reagent, reag. ISO, reag. Ph. Eur., 95.0-97.0%
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Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
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Methanol, ACS reagent, ≥99.8%
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Methanol, BioReagent, ≥99.93%
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Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Methanol, ACS reagent, ≥99.8%
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Sulfuric acid, puriss., meets analytical specification of Ph. Eur., BP, 95-97%
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Ethyl alcohol, Pure, 200 proof, anhydrous, ≥99.5%
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Ethanol, absolute, sales not in Germany, ≥99.8% (vol.)
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Methanol solution, suitable for NMR (reference standard), 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
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Ethyl alcohol, Pure, 190 proof, meets USP testing specifications
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2-Propanol, anhydrous, 99.5%
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2-Propanol, electronic grade, 99.999% trace metals basis
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