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- Identification of gallotannins and ellagitannins in aged wine spirits : a new perspective using alternative ageing technology and high-resolution mass spectrometryPublication . Fernandes, Tiago A.; Antunes, Alexandra M.M.; Caldeira, Ilda; Anjos, O.; Freitas, Victor; Fargeton, Laurent; Boissier, Benjamin; Catarino, Sofia; Canas, SaraThis research was focused on identifying gallotannins and ellagitannins degradation pathways to better understand their behavior in complex media such as wine spirits (WS). A WS was aged with chestnut wood staves with three levels of micro-oxygenation, nitrogen, and using wooden barrels. Gallotannins and ellagitannins were identified by LC-ESI-HRMS/MS using a Q-TOF in samples collected at 8, 21, 60, 180, 270, and 365 days of ageing, allowed comparing their relative abundances according to the ageing technology. It was established for the first time, the importance of oxygen in gallotannins and ellagitannins formation/degradation pathways in WS and shading light into the explanation for the steady increase of gallic and ellagic acid contents on WS during ageing. The results also highlighted the presence of penta-O-galloyl-β-D-glucose, tetra-O-galloyl-β-D-glucose, tri- O-galloyl-β-D-glucose, di-O-galloyl-β-D-glucose, and mono-O-galloyl-β-D-glucose, 2,3-(S)-hexahydroxydiphenoyl-β-D-glucose, pedunculagin, isomers vescalagin/castalagin and two products stemming from ethanol-promoted oxidation of castalagin/vescalagin and vescalin/castalin, in the composition WS aged with chestnut wood.
- Application of functional data analysis and FTIR-ATR spectroscopy to discriminate wine spirits ageing technologiesPublication . Anjos, O.; Martínez Comesaña, Miguel; Caldeira, Ilda; Pedro, Soraia; Eguía Oller, Pablo; Canas, SaraFourier transform infrared spectroscopy (FTIR) with Attenuated Total Reflection (ATR) combined with functional data analysis (FDA) was applied to differentiate aged wine spirits according to the ageing technology (traditional using 250 L wooden barrels versus alternative using micro-oxygenation and wood staves applied in 1000 L stainless steel tanks), the wood species used (chestnut and oak), and the ageing time (6, 12, and 18 months). For this purpose, several features of the wine spirits were examined: chromatic characteristics resulting from the CIELab method, total phenolic index, concentrations of furfural, ellagic acid, vanillin, and coniferaldehyde, and total content of low molecular weight phenolic compounds determined by HPLC. FDA applied to spectral data highlighted the differentiation between all groups of samples, confirming the differentiation observed with the analytical parameters measured. All samples in the test set were differentiated and correctly assigned to the aged wine spirits by FDA. The FTIR-ATR spectroscopy combined with FDA is a powerful methodology to discriminate wine spirits resulting from different ageing technologies.
- Screening of different ageing technologies of wine spirit by application of Near-Infrared (NIR) Spectroscopy and volatile quantificationPublication . Anjos, O.; Caldeira, Ilda; Roque, Rita; Pedro, Soraia; Lourenço, Sílvia; Canas, SaraScreening of different ageing technologies of wine spirit by application of Near-Infrared (NIR) Spectroscopy and volatile quantification.
- Effect of innovative technology using staves and micro-oxygenation on the odorant and sensory profile of aged wine spiritPublication . Soares, Joana Granja; Roque, Rita; Cabrita, M.J.; Anjos, O.; Belchior, A. Pedro; Caldeira, Ilda; Canas, SaraThe aged wine spirit is a beverage with great aromatic complexity. Their volatile compounds with odorant power coming from the distillate and from the wood used in its ageing, and the interactions that take place in the process, enhanced by oxygen, all contribute to this complexity. Due to time and cost inherent of ageing wine spirits in wooden barrels, research has sought to develop more sustainable alternatives to do it. In this context, the present study compares, the effect of traditional (wooden barrel) and alternative system (stainless steel tank with dipped staves and micro-oxygenation), on the odorant and sensory profile of a wine spirit, using Limousin oak and chestnut wood, after 12 months of ageing. The results suggest that the ageing process is accelerated by the alternative ageing technology and the chestnut wood, and the corresponding wine spirits presented characteristics of greater sensory evolution and strong wood compounds extraction.
- Wine spirit ageing with chestnut staves under different micro-oxygenation strategies: effects on the volatile compounds and sensory profilePublication . Caldeira, Ilda; Vitória, Cláudia; Anjos, O.; Fernandes, Tiago A.; Gallardo, Eugenia; Fargeton, Laurent; Boissier, Benjamin; Catarino, Sofia; Canas, SaraThe purpose of this work is to evaluate the wine spirit aged by an alternative process (staves combined with different micro-oxygenation levels) and its comparison with the traditional process (wooden barrels). This evaluation was made by analyzing the volatile compounds and sensory profile of the spirits during 365 days of ageing. The findings confirmed the role played by oxygen in the volatile profile of aged wine spirits. Samples of alternative ageing modalities were well distinguished from those of wooden barrels based on the volatile profile, namely on the concentrations of several volatile phenols. From a sensory point of view, the results are promising with high overall consistency scores obtained from samples of alternative ageing process modalities.
- Phenolic profile and colour acquired by the wine spirit in the beginning of ageing : alternative technology using micro-oxygenation vs traditional technologyPublication . Canas, Sara; Caldeira, Ilda; Anjos, O.; Belchior, A. PedroAlternative technologies have been extensively investigated towards a more sustainable ageing of red wine, but few studies were made on wine spirits. Moreover, the effect of micro-oxygenation on wine spirits’ ageing is still unknown. This work examined the effect of micro-oxygenation and wood staves applied in 1000 L stainless steeltanksversus250 L wooden barrels on the phenolic composition and chromatic characteristics acquired by the wine spirit over the first six months of ageing. Two different kinds of wood, Limousin oak and chestnut, were used. Significantly higher total phenolic content and individual contents of low molecular weight phenolic compounds (syringic acid, ellagic acid, vanillin, syringaldehyde, coniferal dehyde, sinapaldehyde and umbelli-ferone) were obtained with micro-oxygenation and staves than with barrels, for both kinds of wood. Accordingly, greater colour evolution (lower lightness, higher saturation and higher intensities of red, yellow and brown hues) was achieved in the former. These results were ascribed to a faster extraction and its balance with several phenomena involving the wood-derived compounds in the specific environment created by the direct supply of oxygen. A synergistic effect between the alternative technology and the chestnut wood was also observed.
- Micro-oxygenation level as a key to explain the variation in the colour and chemical composition of wine spirits aged with chestnut wood stavesPublication . Canas, Sara; Anjos, O.; Caldeira, Ilda; Fernandes, Tiago A.; Santos, Nádia; Lourenço, Sílvia; Soares, Joana Granja; Fargeton, Laurent; Boissier, Benjamin; Catarino, SofiaA deep knowledge of oxygenation level effect on wine spirits’ ageing is imperative to understand ageing chemistry and to select the most suitable technological option towards quality and sustainability. Following two articles on the same trial, this work focused on colour, total phenolic index (TPI) and basic chemical characteristics of a wine spirit aged in 50 L demijohns with chestnut wood staves together with three micro-oxygenation (MOX) levels. Chromatic characteristics and TPI were monitored over time (8–365 days) while sensory colour, alcoholic strength, acidity, pH and dry extract were assessed at the end of ageing. Results showed that stronger oxygenation promoted significantly faster colour evolution (lower lightness, higher chroma, red, yellow and brown hues) and higher TPI than mild and intermediate oxygenation until 60 days, probably by favouring the leaching of outer wood layers and extraction/degradation of tannins. No significant differences were found between these ageing modalities at 365 days. Outcomes suggest that the stronger MOX is the most suitable modality in terms of quality and sustainability. Significant differences between wine spirits resulting from MOX and control modality (slower colour evolution, lower TPI and dry extract) confirms the oxygen pivotal role in wine spirit’s ageing, particularly in the colour evolution