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A sensitive method for the rapid determination of underivatized ethyl carbamate in fortified wine by liquid chromatography-electrospray tandem mass spectrometry
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Advisor(s)
Abstract(s)
This work presents the optimization of a miniaturized
liquid-liquid extraction (mLLE) followed by reversed-phase
liquid chromatography-electrospray tandem mass spectrometry
(RP-HPLC-MS/MS) for the determination of ethyl carbamate
(EC) in fortified wine, without using derivatizing agents. The
mLLE was optimized by an experimental design. Thus, 15 mL
of wine and 8 mL of ethyl acetate were used for the extraction.
After concentration, each extract was injected into the HPLC MS/MS equipment and the characteristic secondary ion
transition of EC (m/z = 90.10 → 62.05) was used for the quan tification purposes. The proposed method presented a good lin earity (R2 = 0.9999) and a high sensitivity with low limits of
detection (LOD) and quantification (LOQ), 0.17 and
0.52 μg L−1
, respectively. The precision (repeatability and
reproducibility) never exceeded 8% of variation, and the
recoveries varied between 93 and 114%. The applicability of
the method was checked through the analysis of 24 fortified
wines, with EC values ranging between 23 ± 1 and
194 ± 5 μg L−1
. All chromatograms revealed good peak
resolutions. This new method is efficient for the simple, fast,
and reliable determination of EC in fortified wines, providing
great sensitivity without using derivatizing agents or large
volumes of organic solvents.
Description
Keywords
Ethyl carbamate Liquid-liquid extraction Wine Liquid chromatography-mass spectrometry Design of experiments . Faculdade de Ciências da Vida Faculdade de Ciências Exatas e da Engenharia
Citation
Leça, J. M., Pereira, V., Pereira, A. C., & Marques, J. C. (2018). A sensitive method for the rapid determination of underivatized ethyl carbamate in fortified wine by liquid chromatography-electrospray tandem mass spectrometry. Food analytical methods, 11(2), 327-333. DOI 10.1007/s12161-017-1002-3
Publisher
Springer