Sergio Javier Pérez Olivero

A new method for the determination of carbonyl compounds in wines by headspace solid-phase microextraction coupled to gas chromatography-ion trap mass spectrometry.

A new analytical method for the determination of 18 carbonyl compounds [2,3-pentadione, hexanal, (E)-2-hexen-1-al, octanal, acetoin, (E)-2-octenal, furfural, decanal, (E)-2-nonenal, benzaldehyde, 5-methylfurfural, (E,E)-2-cis-6-nonadienal, β-damascenone, phenylacetaldehyde, acetophenone, (E,E)-2,4-decadienal, benzophenone, and vanillin] in wines using automated headspace solid-phase microextraction (HS/SPME) coupled to gas chromatography-ion trap mass spectrometry (GC-ITMS) was developed. Five fibers with different polarities were tested, and a study of the influence of various factors such as time and extraction temperature, desorption time and temperature, pH, and ionic strength and content in tannins, anthocyans, sucrose, SO(2), and alcoholic degree was conducted. These factors were optimized using a synthetic wine doped with the different analytes. The proposed method affords wide ranges of linearity, good linearity (r(2) > 0.998), values of repeatability and reproducibility lower than 5.5% of RSD, and detection limits ranging from 0.62 μg/L for β-damascenone to 129.2 μg/L for acetoin. Therefore, the optimized method was applied to the quantitative analysis of the aforementioned analytes in real samples of wines.

A new method for the determination of short-chain fatty acids from the aliphatic series in wines by headspace solid-phase microextraction-gas chromatography-ion trap mass spectrometry.

A new analytical method for the determination of nine short-chain fatty acids (acetic, propionic, isobutyric, butyric, isovaleric, 2-methylbutyric, hexanoic, octanoic and decanoic acids) in wines using the automated HS/SPME-GC-ITMS technique was developed and optimised. Five different SPME fibers were tested and the influence of different factors such as temperature and time of extraction, temperature and time of desorption, pH, strength ionic, tannins, anthocyans, SO(2), sugar and ethanol content were studied and optimised using model solutions. Some analytes showed matrix effect so a study of recoveries was performed. The proposed HS/SPME-GC-ITMS method, that covers the concentration range of the different analytes in wines, showed wide linear ranges, values of repeatability and reproducibility lower than 4.0% of RSD and detection limits between 3 and 257 μgL(-1), lower than the olfactory thresholds. The optimised method is a suitable technique for the quantitative analysis of short-chain fatty acids from the aliphatic series in real samples of white, rose and red wines.