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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.
- FT-Raman methodology applied to identify different ageing stages of wine spiritsPublication . Anjos, O.; Caldeira, Ilda; Pedro, Soraia; Canas, SaraDuring the ageing process of wine spirits several phenomena occur, which are responsible for the final quality of the beverage. This work aimed to discriminate the aged wine spirits according to the wood species, ageing technology and ageing time using FT-Raman methodology. For this purpose, the same Lourinhã wine distillate aged in 250-L wooden barrels of Limousin oak wood (L) and chestnut wood (C) separately and used together (L + C), was monitored through FT-Raman during the first 12 months of ageing. This technique was also applied to the same wine distillate aged in stainless steel tanks with staves of the same kinds of wood and during the same period. FT-Raman allows separating the wine spirits according to the different wood species and ageing time. This technique seems to be a promising tool to monitor the ageing process of wine spirit through different technologies.
- 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.
- Vibrational spectroscopy applied to Arbutus unedo fruit spirit characterizationPublication . Antunes, Carlos Alberto Lopes; Caldeira, Ilda; Pedro, Soraia; Canas, Sara; Anjos, O.Arbutus unedo spirit (AUS) is a typical beverage of Mediterranean countries, which is usually produced without wood ageing. However, nowadays there is a trend related to the innovation and search for new market options related to this beverage. This work aimed to identify a technique to distinguish the AUS aged with different times and different toasting levels by an easier and cheaper way.
- Variation of extractable compounds and lignin contents in wood fragments used in the aging of wine brandiesPublication . Anjos, O.; Carmona, Clarisse Pires; Caldeira, Ilda; Canas, SaraAging systems of wine brandies have been a target of investigation to reduce the costs and aging time. In this study, the extractives and Klason lignin contents of wood fragments used in the aging of wine brandies in stainless steel tanks were evaluated. Two types of wood fragments, known as staves and tablets, and two wood botanical species, Limousin oak (Quercus robur L. from the Limousin region of France) and Portuguese chestnut (Castanea sativa Mill.), with heavy toasting levels were used. The wood extractive and Klason lignin contents were analyzed before and 30 months after the aging of wine brandy. The results showed that the chestnut wood presented the highest content of extractives, while the Klason and total lignin contents were higher in the oak wood. A highly significant effect from the tablets was found on the extractives and Klason lignin contents, while the soluble lignin content was more affected by the staves. Oxygenation of the wine brandies during the aging process negatively affected the release of extractives and lignin from the wood to the brandy, and therefore will impact the overall quality of the brandy.
- 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.
- Development of blueberry liquor: influence of distillate, sweetener and fruit quantity.Publication . Caldeira, Ilda; Lopes, Daniel; Delgado, Teresa; Canas, Sara; Anjos, O.In this work different formulations of blueberry liquor were tested and characterised based on their physico-chemical and sensory characteristics.