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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
Sulfuric acid, 99.999%
Sigma-Aldrich
Methanol, anhydrous, 99.8%
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Methanol, NMR reference standard
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3-Methyl-2-pentanone, 99%
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Isopropyl alcohol, ≥99.7%, FCC, FG
Supelco
N,N′-Bis(acryloyl)cystamine, BioReagent, suitable for electrophoresis
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
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Methanol, HPLC Plus, ≥99.9%, poly-coated bottles
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Methanol, BioReagent, ≥99.93%
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Sulfuric acid, puriss., meets analytical specification of Ph. Eur., BP, 95-97%
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Methanol, ACS reagent, ≥99.8%
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Methanol, Absolute - Acetone free
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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, ACS reagent, ≥99.8%
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Methanol, ACS spectrophotometric grade, ≥99.9%
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Methanol, ACS reagent, ≥99.8%
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Methanol, Laboratory Reagent, ≥99.6%
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Sulfuric acid solution, puriss. p.a., ≥25% (T)
Sigma-Aldrich
Sulfuric acid, ACS reagent, 95.0-98.0%
Sigma-Aldrich
Methanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
Methanol, puriss., meets analytical specification of Ph Eur, ≥99.7% (GC)
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Formic acid, puriss. p.a., ACS reagent, reag. Ph. Eur., ≥98%