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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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Abstract

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 quantification purposes. The proposed method presented a good linearity (R 2 = 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.

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Abbreviations

EC:

Ethyl carbamate

mLLE:

Miniaturized liquid-liquid extraction

LC:

Liquid chromatography

MS/MS:

Tandem mass spectrometry

MRM:

Multiple reaction-monitoring

FW:

Fortified wine

DoE:

Design of experiments

IS:

Internal standard

ME:

Matrix effect

LOD:

Limit of detection

LOQ:

Limit of quantification

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Authors and Affiliations

  1. Faculty of Exact Sciences and Engineering, University of Madeira, Campus da Penteada, 9020-105, Funchal, Portugal

    João M. Leça, Vanda Pereira, Ana C. Pereira & José C. Marques

  2. Institute of Nanostructures, Nanomodelling and Nanofabrication (I3N), University of Aveiro, Aveiro, Portugal

    João M. Leça, Vanda Pereira & José C. Marques

  3. CIEPQPF, Department of Chemical Engineering, University of Coimbra, Pólo II - Rua Sílvio Lima, 3030-790, Coimbra, Portugal

    Ana C. Pereira

Authors
  1. João M. Leça
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  2. Vanda Pereira
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  3. Ana C. Pereira
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  4. José C. Marques
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Corresponding author

Correspondence to Vanda Pereira.

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Funding

João M. Leça (PhD studentship), Vanda Pereira (Post Doc fellowship), and Ana C. Pereira (Post Doc fellowship) are thankful to the Agência Regional para o Desenvolvimento da Investigação Tecnologia e Inovação for the financial support through their grants in the scope of the project M1420-09-5369-FSE-000001. The financial support was given by Fundo Europeu de Desenvolvimento Regional (+ Conhecimento program, VALIMED project, MADFDR-01-0224-FEDER-000006).

Conflict of Interest

João M. Leça declares that he has no conflict of interest. Vanda Pereira declares that she has no conflict of interest. Ana C. Pereira declares that she has no conflict of interest. José C. Marques declares that he has no conflict of interest.

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This article does not contain any studies with human or animal subjects.

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Leça, J.M., Pereira, V., Pereira, A.C. et al. A Sensitive Method for the Rapid Determination of Underivatized Ethyl Carbamate in Fortified Wine by Liquid Chromatography-Electrospray Tandem Mass Spectrometry. Food Anal. Methods 11, 327–333 (2018). https://doi.org/10.1007/s12161-017-1002-3

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  • DOI: https://doi.org/10.1007/s12161-017-1002-3

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