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

摘要

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 (GCxGC/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 (D-2) of GCxGC/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 1.5gL(-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 (0.6gL(-1)). Acetaldehyde (19.9 to 44.0gL(-1)) and furfural (1.1 to 6.9gL(-1)) were found in all samples. Acrolein was detected in 75% of samples in levels ranging from 0.7 to 50.2gL(-1).