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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-12C, 99.95 atom % 12C
Sigma-Aldrich
Methanol solution, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
2-Propanol, BioReagent, ≥99.5%
Sigma-Aldrich
2-Propanol, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Ethanol, purum, secunda spirit, denaturated with 2% 2-butanone, S15, ~96% (based on denaturant-free substance)
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Ammonium hydrogen difluoride, 99.999% trace metals basis
Sigma-Aldrich
2-Propanol, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
Sigma-Aldrich
Ethanol, purum, absolute ethanol, denaturated with 2% 2-butanone, A15 MEK1, ≥99.8% (based on denaturant-free substance)
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Isopropyl alcohol, meets USP testing specifications
Sigma-Aldrich
2-Propanol, Laboratory Reagent, ≥99.5%
Sigma-Aldrich
Ethyl alcohol, Pure 200 proof
Sigma-Aldrich
2-Propanol, ACS reagent, ≥99.5%
Sigma-Aldrich
Ethyl alcohol, Pure, 200 proof, ACS reagent, ≥99.5%
Sigma-Aldrich
2-Propanol, puriss. p.a., ACS reagent, ≥99.8% (GC)
Sigma-Aldrich
Ethanol, purum, fine spirit, denaturated with 2% 2-butanone, F25 MEK1, ~96% (based on denaturant-free substance)
Sigma-Aldrich
Ethanol, purum, fine spirit, denaturated with 4.8% methanol, F25 METHYL1, ~96% (based on denaturant-free substance)
Sigma-Aldrich
Formic acid, ACS reagent, ≥88%
Sigma-Aldrich
Ethyl alcohol, Pure, 160 proof, Excise Tax-free, Permit for use required
Sigma-Aldrich
Ammonium hydrogen difluoride, reagent grade, 95%
Sigma-Aldrich
Ethyl alcohol, Pure, 200 proof, meets USP testing specifications
Sigma-Aldrich
Methanol
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Supelco
N,N′-Bis(acryloyl)cystamine, BioReagent, suitable for electrophoresis
Sigma-Aldrich
3-Methyl-2-pentanone, 99%
Sigma-Aldrich
Sulfuric acid, 99.999%
Sigma-Aldrich
Isopropyl alcohol, ≥99.7%, FCC, FG
Sigma-Aldrich
Sulfuric acid, puriss., meets analytical specification of Ph. Eur., BP, 95-97%