Development of a Method for Determination of Target Toxic Carbonyl Compounds in Must and Wine Using HS-SPME-GC/MS-SIM After Preliminary GC×GC/TOFMS Analyses


A gas chromatography with mass spectrometric detection in selected ion monitoring mode (GC/qMS-SIM) method, preceded by comprehensive two-dimensional gas chromatography with a time-of-flight mass spectrometric detector (GC×GC/TOFMS) analyses to identify possible coelutions, was validated for the simultaneous determination of formaldehyde, acetaldehyde, acrolein, furfural, and ethyl carbamate in must and wines. Derivatized acetaldehyde and acrolein coeluted with other compounds and were resolved in the second chromatographic dimension (2D) of GC×GC/TOFMS. The most intense ions of the mass spectra of the analytes that were not present in the mass spectra of interfering compounds were used in GC/qMS-SIM. Figures of merit demonstrated the appropriateness of the developed GC/qMS-SIM method, including recovery (90–102%), relative standard deviation obtained in repeatability, and precision assays that were lower than 9 and 12%, respectively. Limits of detection and quantification for all compounds demonstrated the adequate sensitivity of the method for the quantification of carbonyl compounds (values lower than 0.8 and 1.5 μg L−1, respectively). Results confirmed that furan-containing compounds may be impartially analyzed using HS-SPME-qGC/MS without interference of artifact formation during extraction/desorption. In addition, the importance of adjusting ethanol content according to the level of ethanol in samples has been demonstrated. Ethyl carbamate was not detected in analyzed samples, while formaldehyde was found in levels lower than LOQ (0.6 μg L−1). Acetaldehyde (19.9 to 44.0 μg L−1) and furfural (1.1 to 6.9 μg L−1) were found in all samples. Acrolein was detected in 75% of samples in levels ranging from 0.7 to 50.2 μg L−1.

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This study was funded by the National Council of Technological and Scientific Development (Conselho Nacional de Desenvolvimento Científico e Tecnológico, CNPq. Project BJT 401581/2014-4; CNPq project Pq 306067/2016-1), the Coordination for the Improvement of Higher Education Personnel (Coordenação de Aperfeiçoamento de Pessoal de Nível Superior, CAPES), and Research Support Foundation of Rio Grande do Sul (Fundação de Amparo à Pesquisa do Estado do Rio Grande do Sul, FAPERGS, Edital Pesquisador Gaúcho, Project 1995-2551/13-7).

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Correspondence to Juliane Elisa Welke.

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Daiani F. Cecchin declares that she has no conflict of interest. Karolina C. Hernandes declares that she has no conflict of interest. Karine P. nicolli declares that she has no conflict of interest. Érica A. Souza-Silva declares that she has no conflict of interest. Vitor Manfroi declares that he has no conflict of interest. Claudia A. Zini declares that she has no conflict of interest. Juliane Elisa Welke declares that she has no conflict of interest.

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Ferreira, D.C., Hernandes, K.C., Nicolli, K.P. et al. Development of a Method for Determination of Target Toxic Carbonyl Compounds in Must and Wine Using HS-SPME-GC/MS-SIM After Preliminary GC×GC/TOFMS Analyses. Food Anal. Methods 12, 108–120 (2019).

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  • Vinification
  • GC/qMS
  • Toxic compounds
  • Comprehensive two-dimensional gas chromatography