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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.
- PLS-R calibration models for wine spirit volatile phenols prediction by Near-Infrared SpectroscopyPublication . Anjos, O.; Caldeira, Ilda; Fernandes, Tiago A.; Pedro, Soraia; Vitória, Cláudia; Alves, Sheila Oliveira; Catarino, Sofia; Canas, SaraNear-infrared spectroscopic (NIR) technique was used, for the first time, to predict volatile phenols content, namely guaiacol, 4-methyl-guaiacol, eugenol, syringol, 4-methyl-syringol and 4- allyl-syringol, of aged wine spirits (AWS). This study aimed to develop calibration models for the volatile phenol’s quantification in AWS, by NIR, faster and without sample preparation. Partial least square regression (PLS-R) models were developed with NIR spectra in the near-IR region (12,500–4000 cm−1 ) and those obtained from GC-FID quantification after liquid-liquid extraction. In the PLS-R developed method, cross-validation with 50% of the samples along a validation test set with 50% of the remaining samples. The final calibration was performed with 100% of the data. PLS-R models with a good accuracy were obtained for guaiacol (r2 = 96.34; RPD = 5.23), 4-methyl-guaiacol (r2 = 96.1; RPD = 5.07), eugenol (r2 = 96.06; RPD = 5.04), syringol (r2 = 97.32; RPD = 6.11), 4-methylsyringol (r2 = 95.79; RPD = 4.88) and 4-allyl-syringol (r2 = 95.97; RPD = 4.98). These results reveal that NIR is a valuable technique for the quality control of wine spirits and to predict the volatile phenols content, which contributes to the sensory quality of the spirit beverages.
- Study of odorant compounds and sensory changes associated with wine spirit ageing using chestnut wood and Limousin oak under different technologiesPublication . Caldeira, Ilda; Anjos, O.; Vitória, Cláudia; Fernandes, Tiago A.; Catarino, Sofia; Canas, SaraWine spirit, resulting from wine distillation, usually undergoes ageing in wood before being marketed. Traditionally, the oak wood, especially from the French region of Limousin (mostly Quercus robur L.), is used for manufacturing the barrels for this purpose.
- PLS-R calibration models for wine spirit volatile phenols prediction by Near-Infrared SpectroscopyPublication . Anjos, O.; Caldeira, Ilda; Fernandes, Tiago A.; Pedro, Soraia; Vitória, Cláudia; Alves, Sheila Oliveira; Catarino, Sofia; Canas, SaraNear-infrared spectroscopic (NIR) technique was used, for the first time, to predict volatile phenols content, namely guaiacol, 4-methyl-guaiacol, eugenol, syringol, 4-methyl-syringol and 4-allyl-syringol, of aged wine spirits (AWS). This study aimed to develop calibration models for the volatile phenol’s quantification in AWS, by NIR, faster and without sample preparation. Partial least square regression (PLS-R) models were developed with NIR spectra in the near-IR region (12,500–4000 cm1) and those obtained from GC-FID quantification after liquid-liquid extraction. In the PLS-R developed method, cross-validation with 50% of the samples along a validation test set with 50% of the remaining samples. The final calibration was performed with 100% of the data. PLS-R models with a good accuracy were obtained for guaiacol (r2 = 96.34; RPD = 5.23), 4-methyl-guaiacol (r2 = 96.1; RPD = 5.07), eugenol (r2 = 96.06; RPD = 5.04), syringol (r2 = 97.32; RPD = 6.11), 4-methylsyringol (r2 = 95.79; RPD = 4.88) and 4-allyl-syringol (r2 = 95.97; RPD = 4.98). These results reveal that NIR is a valuable technique for the quality control of wine spirits and to predict the volatile phenols content, which contributes to the sensory quality of the spirit beverages.
- Influence of the storage in bottle on the antioxidant activities and related chemical characteristics of wine spirits aged with chestnut staves and micro-oxygenationPublication . Alves, Sheila Oliveira; Lourenço, Sílvia; Anjos, O.; Fernandes, Tiago A.; Caldeira, Ilda; Catarino, Sofia; Canas, SaraDifferent ageing technology of wine spirits (WSs) has been investigated, but little has been published on the chemical evolution of aged WS during storage in bottle. The purpose of this study was to examine how 12 months of storage in bottle affected the evolution of antioxidant activity (DPPH, FRAP and ABTS assays), total phenolic index (TPI) and low molecular weight (LMW) compounds content of the WSs aged through alternative technology using three micro-oxygenation levels (MOX) and nitrogen control (N). Results revealed the ability of phenolic compounds from aged WSs to scavenge free radicals during storage in bottle. Among the in vitro antioxidant-activity methods, FRAP assay was the more effective to differentiate WSs according to the ageing technology. Concerning the overall influence of storage in bottle on antioxidant activity, and TPI and LMW compounds content, the higher results were obtained for the MOX modalities (O15, O30 and O60), which showed a similar evolution. In summary, this study provides innovative information, demonstrating that the differences between the aged WSs imparted throughout the ageing process (resulting from different MOX levels) were mostly retained, and only slight modifications during storage in bottle were found.
- Casting light on the chemical characterization of acacia podsPublication . Pedro, Soraia; Fernandes, Tiago A.; Antunes, Alexandra M.M.; Gominho, Jorge; Gallardo, Eugenia; Anjos, O.Invasive species impose a strain on natural ecosystems by contributing to the loss of certain native species. Acacia species are amongst the most aggressive invasive species in Portugal. In this work, Acacia retinodes, A. longifolia, A. melanoxylon, A. pycnantha and A. dealbata pods were studied concerning the extraction of compounds for potential industrial application.
- The effect of transition metals on coniferaldehyde oxidation in wine spirits model solutionsPublication . Alves, Sheila Oliveira; Lourenço, Sílvia; Fernandes, Tiago A.; Anjos, O.; Caldeira, Ilda; Catarino, Sofia; Canas, SaraWood is known to be a complex biological system composed mainly of cellulose, hemicelluloses and lignin. Cellulose is commonly degraded by the thermal treatment of wood during coopering giving rise to HMF and 5- methylfurfural, while hemicellulose can generate pentose by hydrolysis, and posteriorly, furfural and its derivatives. Lignin transformations during ageing process of distillates are among the most important factors that may influence the quality of aged wine spirit (WS).
- First chemical profile analysis of acacia podsPublication . Pedro, Soraia; Fernandes, Tiago A.; Luís, Ângelo; Antunes, Alexandra M.M.; Gonçalves, José Carlos; Gominho, Jorge; Gallardo, Eugenia; Anjos, O.This study intended to evaluate the potential industrial applications of various Acacia species (Acacia melanoxylon, Acacia longifolia, Acacia cyclops, Acacia retinodes, Acacia pycnantha, Acacia mearnsii, and Acacia dealbata) by examining their chemical composition, antioxidant, and antimicrobial properties. Using high-resolution mass spectrometry, a comprehensive analysis successfully identified targeted compounds, including flavonoids (flavonols/flavones) and phenolic acids, such as 4-hydroxybenzoic acid, p-coumaric acid, and ellagic acid. Additionally, p-coumaric acid was specifically identified and quantified within the hydroxycinnamic aldehydes. This comprehensive characterization provides valuable insights into the chemical profiles of the studied species. Among the studied species, A. pycnantha exhibited a higher concentration of total phenolic compounds, including catechin, myricetin, quercetin, and coniferaldehyde. Furthermore, A. pycnantha displayed notable antibacterial activity against K. pneumoniae, E. coli, S. Typhimurium, and B. cereus. The identified compounds in Acacia pods and their shown antibacterial activities exhibit promising potential for future applications. Moreover, vibrational spectroscopy was a reliable method for distinguishing between species. These significant findings enhance our understanding of Acacia species and their potential for various industrial applications.
- Application of near-infrared spectroscopy to characterize volatile phenols and sensory profile of aged wine spiritsPublication . Anjos, O.; Caldeira, Ilda; Fernandes, Tiago A.; Pedro, Soraia; Vitória, Cláudia; Alves, Sheila Oliveira; Catarino, Sofia; Canas, SaraVolatile phenols are low molecular weight aromatic alcohols, with particular importance in wine spirits aged with wood due to their strong influence on sensory profile.
- 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.
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