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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, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
2-Propanol, BioUltra, for molecular biology, ≥99.5% (GC)
Sigma-Aldrich
Ethanol, purum, secunda spirit, denaturated with 2% 2-butanone, S15, ~96% (based on denaturant-free substance)
Sigma-Aldrich
Ethyl alcohol, Pure, 190 proof, ACS spectrophotometric grade, 95.0%
Sigma-Aldrich
2-Propanol, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%, poly coated bottles
Sigma-Aldrich
2-Propanol, for molecular biology, BioReagent, ≥99.5%
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Methanol solution, (Methanol:Dimethyl sulfoxide 1:1 (v/v))
Sigma-Aldrich
2-Propanol, electronic grade, 99.999% trace metals basis
Sigma-Aldrich
2-Propanol, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)
Sigma-Aldrich
2-Propanol, puriss. p.a., ACS reagent, ≥99.8% (GC)
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Ammonium hydrogen difluoride, 99.999% trace metals basis
Sigma-Aldrich
2-Propanol, puriss., meets analytical specification of Ph. Eur., BP, USP, ≥99.5% (GC)
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Ethyl alcohol, Pure, 200 proof, ACS reagent, ≥99.5%
Sigma-Aldrich
Ethanol, ACS reagent, prima fine spirit, without additive, F15 o1
Sigma-Aldrich
Formic acid, ≥95%, FCC, FG
Sigma-Aldrich
Formic acid, puriss., meets analytical specifications of DAC, FCC, 98.0-100%
Sigma-Aldrich
2-Propanol, ACS reagent, ≥99.5%
Sigma-Aldrich
Formic acid, ACS reagent, ≥96%
Sigma-Aldrich
Isopropyl alcohol, meets USP testing specifications
Sigma-Aldrich
Formic acid, ACS reagent, ≥88%
Sigma-Aldrich
Ethyl alcohol, Pure 200 proof, for molecular biology
Sigma-Aldrich
Formic acid, reagent grade, ≥95%
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Ammonium hydrogen difluoride, reagent grade, 95%
Sigma-Aldrich
Ethanol, purum, absolute ethanol, denaturated with 1% cyclohexane, A15 CYCLO1, ≥99.8% (based on denaturant-free substance)
Sigma-Aldrich
Ethanol, purum, fine spirit, denaturated with 2% 2-butanone, F25 MEK1, ~96% (based on denaturant-free substance)
Sigma-Aldrich
Ethanol, purum, absolute ethanol, denaturated with 2% 2-butanone, A15 MEK1, ≥99.8% (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
2-Propanol, Laboratory Reagent, ≥99.5%
Sigma-Aldrich
Ethanol, purum, absolute ethanol, denaturated with 4.8% isopropanol, A15 IPA1, ≥99.8% (based on denaturant-free substance)