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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, Absolute - Acetone free
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
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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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Methanol, ACS reagent, ≥99.8%
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Methanol, BioReagent, ≥99.93%
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Methanol, Laboratory Reagent, ≥99.6%
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Methanol, NMR reference standard
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Sulfuric acid, 99.999%
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3-Methyl-2-pentanone, 99%
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
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Isopropyl alcohol, ≥99.7%, FCC, FG
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N,N′-Bis(acryloyl)cystamine, BioReagent, suitable for electrophoresis
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Sulfuric acid, puriss., meets analytical specification of Ph. Eur., BP, 95-97%
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Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
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2-Propanol, electronic grade, 99.999% trace metals basis
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Ammonium hydrogen difluoride, 99.999% trace metals basis
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2-Propanol, BioUltra, for molecular biology, ≥99.5% (GC)
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Formic acid, ≥95%, FCC, FG
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Methanol-12C, 99.95 atom % 12C
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2-Propanol, for molecular biology, BioReagent, ≥99.5%
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Formic acid, reagent grade, ≥95%
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Formic acid, ACS reagent, ≥96%
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Isopropyl alcohol, meets USP testing specifications
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2-Propanol, Laboratory Reagent, ≥99.5%
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2-Propanol, ACS reagent, ≥99.5%
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Ethyl alcohol, Pure, 200 proof, meets USP testing specifications
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Formic acid, ACS reagent, ≥88%
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Ethyl alcohol, Pure, 200 proof, ACS reagent, ≥99.5%