Wine Aging Research Articles

Qualitative Factor-Based Comparison of NMR, Targeted and Untargeted GC-MS and LC-MS on the Metabolomic Profiles of Rioja and Priorat Red Wines.

Wine origin and ageing are two factors related to wine quality which in turn is associated to wine metabolome. Currently, new metabolomic techniques and proper statistics procedures allow accurate profiling of wine metabolome. Thus, the main goal was to evaluate different metabolomic methodologies on their ability to provide patterns on the wine metabolome based on selected factors, such as ageing of barrel-aged wine (factor time), prior usage of the barrels (factor barrel-type), and differences between wine ageing in barrels or glass bottles (factor bottled-wine). In the current study, we implement NMR, targeted and untargeted GC-MS and LC-MS metabolomic analytical techniques so as to gain insights into the volatile and nonvolatile wine metabolome composition of red wines from two cellars located in the only two Spanish Qualified Appellations of Origin; DOQ Priorat and DOCa Rioja regions. Overall, 95 differentially significant metabolites were identified facilitating the evaluation of the analytical methodologies performance and finding common trends of those metabolites depending on the considered factor. The results did not favor NMR as an effective technique on the current dataset whereas suggested LC-MS as an adequate technique for revealing differences based on the factor time, targeted GC-MS on the factor barrel-type, and untargeted GC-MS on the factor bottled-wine. Thus, a combination of different metabolomic techniques is necessary for a complete overview of the metabolome changes. These results ease the selection of the correct methodology depending on the specific factor investigated.

Microventilation system improves the ageing conditions in existent wine cellars

Background and Aims The importance of indoor environmental conditions in a cellar is well known and continuously investigated. The process of wine ageing consists of several steps, during which temperature (T) and relative humidity (RH) play a fundamental role as the quality of the final product is strongly related to stable and suitable environmental conditions. Critical factors, such as mould growth or wine evaporation, have emerged when ventilation has proved to be insufficient or poorly designed. The limitation of stagnant areas and the homogeneity inT and RH provide for proper wine conservation; however, unwanted local conditions can occur in the zones with insufficient air exchange. Methods and Results Considering these aspects, a controlled microventilation and monitoring system was installed in a case study cellar, and T and RH were monitored for 1 year. The data have been analysed to investigate criticalities of the environmental conditions. The ventilation was activated in specific critical conditions to increase the homogeneity of the T and RH in the critical zones. The results show that the microventilation system improves the homogeneity of both T and RH without affecting the average values. Conclusions The study demonstrated the efficacy of the system and indicated possible modifications to improve system performance. Significance of the Study The system proved to be a useful tool for both improving the environmental conditions and providing useful information to the winemakers about the ageing conditions.

Impact of 5-year bottle aging under controlled oxygen exposure on sulfur dioxide and phenolic composition of tannin-rich red wines

Aim: This study aims at understanding the impact of the initial phenolic composition on the evolution of red wines after long bottle aging.Materials and results: three different red wines rich in tannins, Aglianico, Casavecchia and Pallagrello, bottled with the same amount of total sulfur dioxide and different amounts of free sulfur dioxide, were analysed after 5 years of bottle aging under controlled exposure to oxygen passing through the closure. Acetaldehyde and monomeric anthocyanins were determined by HPLC, the chromatic characteristics and the main phenolic classes by spectrophotometry, the saliva precipitation index (SPI) by CHIP electrophoresis, and the astringency subqualities by sensory analysis. The results confirmed that during aging there is an increase in polymerisation reactions. A higher amount of acetaldehyde was detected in wines which were bottled with a lower content of free SO2 and were less rich in anthocyanins and tannins; a significant closure effect was observed for these wines. Regarding the influence of closure on tannins, significant slight differences in vanilline reactive flavans and SPI content were observed for Pallagrello wines only, which were characterised by higher values for tannins at bottling. Astringency subqualities differed with closures for each wine.Conclusion: this study indicates that the amount of initial free and combined sulfur dioxide, as well as that of anthocyanins and tannins, are key factors in driving polymerisation reactions and the aging of red wines. After five years of bottle aging the influence of closure could still be observed.Significance of the study: this study provides new insights into the parameters that need to be evaluated before bottling in order to avoid the wrong evolution of red wines after long bottle aging.

High-Throughput Sequencing Approach to Analyze the Effect of Aging Time and Barrel Usage on the Microbial Community Composition of Red Wines.

Wine aged in barrels or bottles is susceptible to alteration by microorganisms that affect the final product quality. However, our knowledge of the microbiota during aging and the factors modulating the microbial communities is still quite limited. The present work uses high-throughput sequencing (HTS) techniques to deal with the meta-taxonomic characterization of microbial consortia present in red wines along 12 months aging. The wines obtained from two different grape varieties were aged at two different cellars and compared based on time of wine aging in the barrels, previous usage of the barrels, and differences between wine aging in oak barrels or glass bottles. The aging in barrels did not significantly affect the microbial diversity but changed the structure and composition of fungal and bacterial populations. The main microorganisms driving these changes were the bacterial genera Acetobacter, Oenococcus, Lactobacillus, Gluconobacter, Lactococcus, and Komagataeibacter and the fungal genera Malassezia, Hanseniaspora, and Torulaspora. Our results showed that the oak barrels increased effect on the microbial diversity in comparison with the glass bottles, in which the microbial community was very similar to that of the wine introduced in the barrels at the beginning of the aging. Furthermore, wine in the bottles harbored higher proportion of Lactobacillus but lower proportion of Acetobacter. Finally, it seems that 1 year of previous usage of the barrels was not enough to induce significant changes in the diversity or composition of microbiota through aging compared with new barrels. This is the first meta-taxonomic study on microbial communities during wine aging and shows that the microorganism composition of barrel-aged wines was similar at both cellars. These results hint at the possibility of a common and stable microbiota after aging in the absence of exogenous alterations. Further corroborations on the current outcome would be valuable for the comparison and detection of microbial alterations during aging that could potentially prevent economic losses in the wine industry.

Effect of antioxidant supplementation on the polysulfides of white wines

Sulfur chemistry remains one of the most intriguing and elusive fields in wine science. In particular, the possibility for symmetric and asymmetric glutathionylated and cysteinylated polysulfides to act as latent reservoirs for H2S warrants new research on the factors influencing the formation and accumulation of these molecules.The present research studies the impact of pre-fermentative additions of commonly employed antioxidants: glutathione, ascorbic acid, and ellagic tannin. Musts from four different white grape varieties (Riesling, Pinot gris, Pinot blanc, and Johanniter) were analysed using our comprehensive HPLC-HRMS method. Seven symmetric and asymmetric glutathionylated (G) and cysteinylated (C) polysulfides (GS2C, GS3C, GS4C, GS3G, GS4G, CS3C, and CS4C) were detected in the final 48 wine samples. Finally, this work describes for the first time the impact of an accelerated ageing of wine on the polysulfides present. All variables (Must, Treatment, and Time) were shown to impart statistically significant effects (p = 0.0001) in the PERMANOVA model. The PCAs based on polysulfides present in young and aged wine explained more than 80% of the total variance for each grape variety and showed that Asc or GSH additions have tend to produce lower levels of polysulfides in the resultant wines.

Wine Aging Technology: Fundamental Role of Wood Barrels.

The aging of wines is a process used to preserve wine but also to enhance its properties. It is a process of great interest, mainly because of the additional properties it adds to wines and because of its economic implications. Historically, barrels have been employed for centuries for preserving and aging wine due to their resistance and relative impermeability. In general terms, the wine aging process can be divided into two phases: oxidative and reductive aging. Oxidative aging traditionally takes place in barrels while reductive phase occurs in the bottle. During both processes, oxygen plays a fundamental role as well as other factors, for instance: temperature, light, bottle position, microbial growth or storage time. Likewise, during the aging process, a series of chemical reactions take place influencing the composition and organoleptic profile of wine. At this point, oxidative aging in barrels is a fundamental step. Barrels are directly involved in the produced changes on wine’s composition due to the transference of oxygen and phenolic and aromatic compounds from wood to wine. This way, barrels act as an active vessel capable of releasing compounds that affect and improve wine’s characteristics. Regarding, the importance of barrels during aging process, some attention must be given to the species most used in cooperage. These species are conventionally oak species, either French or American. However, other non-conventional species are currently being studied as possible wood sources for the production of wines, such as chestnut robinia or other oak species. In the last decades, new approaches have been developed for barrel aging to find new alternatives more suitable, affordable and feasible to sanitize the process, such as other materials different from wood or the use of wood chips, which is regulated since 2006 by the EU. However, even though some of them have shown promising data, barrels are currently the most used technology for the oxidative stage of table wines aging.

Targeted metabolomics of anthocyanin derivatives during prolonged wine aging: Evolution, color contribution and aging prediction

Anthocyanin derivatives and chromatic characteristics of 234 different-vintage red wine were investigated based on a targeted HPLC-MS/MS and CIELAB approach. The K-means cluster analysis showed that the evolution pattern varies amongst anthocyanin derivative classes. Their stabilities are: pinotins > flavanyl-pyranoanthocyanins, vitisin A > monomeric anthocyanin, direct anthocyanin-flavan-3-ols condensation products > vitisin B, anthocyanin ethyl-linked flavan-3-ols products. The proportion of most pyranoanthocyanins becomes more significant among all detected anthocyanin derivatives during wine aging, whereas flavanols-related anthocyanin derivatives (except for flavanyl-pyranoanthocyanins) decreased drastically. PLSR showed that aging tawny characteristics is related to pyranoanthocyanins except for vitisin B, especially pinotins, whereas monomeric anthocyanins and flavanol-related derivates (except for flavanyl-pyranoanthocyanins) contribute to red violet color. But aging color density is more associated with the content of vitisin A and flavanyl-pyranoanthocyanins. Two predictive models based on random forest and support vector machine modeling showed good performance in predicting the extent of wine aging.

Phenolic and Aroma Changes of Red and White Wines during Aging Induced by High Hydrostatic Pressure.

The aim of this study was to investigate use of high hydrostatic pressure (HHP) along with different antioxidants (glutathione and SO2) as an alternative method for wine preservation and production of low-SO2 wines. In the first phase of the study, low-SO2, young red and white wines were pressurized at three pressure levels (200, 400 and 600 MPa) for 5, 15 and 25 min at room temperature, and analyzed immediately after treatments. Additionally, for the wine aging experiment, red and white wines with standard-SO2, low-SO2+glutathione and low-SO2 content were treated with HHP treatment (200 MPa/5 min) and stored for 12 months in bottles. Color parameters, phenolic and aroma compounds were determined. The sensory evaluation was also conducted. HHP showed very slight, but statistically significant changes in the chemical composition of both red and white wine right after the treatment, and the main variations observed were related to the different pressures applied. Furthermore, during aging, most of the differences observed in chemical composition of pressurized wines, both red and white, were statistically significant, and greater in wines with a lower content of antioxidants. However, after 12 months of aging, some differences between unpressurized and pressurized samples with standard SO2 content were lost, primarily in aroma compounds for red wine and in color and phenolics for white wine. Additionally, similar values were obtained for mentioned characteristics of red and white wines in pressurized samples with standard SO2 and low SO2+glutathione, indicating that HHP in combination with glutathione and lower doses of SO2 might potentially preserve wine. The sensory analysis confirmed less pronounced changes in the sensory attributes of pressurized wines with higher concentration of antioxidants. Furthermore, the treatments applied had a slightly higher effect on the sensory properties of white wine.

Red Wine Oxidation: Accelerated Ageing Tests, Possible Reaction Mechanisms and Application to Syrah Red Wines.

Wine oxidation and ageing involve many complex chemical pathways and reaction mechanisms. The purpose of this study is to set up new and reproducible accelerated red wine ageing tests and identify chemical oxidation or ageing molecular markers. Three accelerated and reproducible ageing tests were developed: a heat test (60 °C); an enzymatic test (laccase test; a chemical test (hydrogen peroxide test). Depending on the test, oxygen consumption was significantly different. For a young wine (2018), the oxygen consumption rate moved from 2.40 ppm·h−1 for the heat test to 3.33 ppm·h−1 for the enzymatic test and 2.86 ppm·h−1 for the chemical test. Once applied to two other vintages (2010 and 2014) from the same winery, the tests revealed different comportments corresponding to wine natural evolution. High resolution UPLC-MS was performed on forced ageing samples and compared to naturally aged red wines. Specific oxidation or ageing ion markers were found with significant differences between tests, revealing the specificity of each test and different possible molecular pathways involved. The hydrogen peroxide test seems to be closer to natural oxidation with an important decrease in absorbance at 520 nm and similar molecular ion variations for [M+H]+ = 291, 331, 347, 493, 535, 581, 639 Da.

Loss oftrans‐resveratrol during storage and ageing of red wines

Background and Aims The concentration of free trans-resveratrol in wine is expected to increase with storage because of hydrolysis of piceid (a bound form of resveratrol). This study measured resveratrol concentration in 16 Australasian red wines ranging from 1 to 6 years old, both initially and after a storage period of 16 months under ambient conditions. Methods and Results During the study period, trans-resveratrol concentration decreased by an average of 76%. The decay in trans-resveratrol was first order over the tested range of wine source and vintage, with a mean trans-resveratrol bottle-storage half-life of 8 (±1 SD) months. Decay rate was remarkably independent of growing condition and year. Conclusion The data suggest isomerisation of trans- to cis-resveratrol via residual enzymatic activity (rather than being catalysed by light or acid). Significance of the Study In general, this may reduce the anticipated health benefits of the wine given that cis-resveratrol displays fewer health benefits than the trans isomer.

Artificial Intelligence Methods for Constructing Wine Barrels with a Controlled Oxygen Transmission Rate.

Oxygen is an important factor in the wine aging process, and the oxygen transmission rate (OTR) is the parameter of the wood that reflects its oxygen permeation. OTR has not been considered in the cooperage industry yet; however, recent studies proposed a nondestructive method for estimating the OTR of barrel staves, but an efficient method to combine these staves to build barrels with a desired OTR is needed to implement it in the industry. This article proposes artificial intelligence methods for selecting staves for the construction of barrel heads or bodies with a desired target OTR. Genetic algorithms were used to implement these methods in consideration of the known OTR of the staves and the geometry of the wine barrels. The proposed methods were evaluated in several scenarios: homogenizing the OTR of the actual constructed barrels, constructing low-OTR and high-OTR barrels based on a preclassification of the staves and implementing the proposed method in real cooperage conditions. The results of these experiments suggest the suitability of the proposed methods for their implementation in a cooperage in order to build controlled OTR barrels.

The impact of ultrasonic treatment on blueberry wine anthocyanin color and its In-vitro anti-oxidant capacity

Ultrasound (US) has been recognized as a non-thermal technology for accelerating blueberry wine aging for flavor development. However, influence of US on anthocyanin and color characteristics is uncertain. In this study, US was applied to new blueberry wine, and changes in color characteristics, anthocyanin content and anti-oxidant capacity were evaluated at early stage of aging period. Low-frequency power US resulted in an improvement in color characteristics and lower chromatic aberration as compared to untreated samples, specially at condition of 180 W, 20 min and 2 cycles. Furthermore, this contribution was attributed to unattenuated anthocyanins protected from US stress. Importantly, the structural polarity dependence was mediated by the impact of US on anthocyanins. Additionally, anti-oxidant activity of blueberry wine was not adversely affected under a moderate US condition. US treatment of blueberry wine was therefore considered to significantly enhance the color presentation, hinting at the possibility of promoting blueberry wine aging.

Study on factors affecting pomegranate (Punica granatum) wine fermentation

Pomegranate fruit has attracted a great attention owing to its phytochemical constituents and its juice fermented as a mild alcoholic drink with availabe bioactive compounds. Therefore, this study was conducted during 2019 at Labone Scientific Co. Ltd, Vietnam with an aim to examine various variables such as the pectinase concentration and treatment duration for juice extraction, the yeast ratio inculation for wine fermentation and the secondary fermentation as aging quality of wine. Pomegranate extract was treated with pectinase enzyme at a concentration of 0.15, 0.20, 0.25 and 0.30% under different duration of 15, 30, 45 and 60 minutes and inoculated with Saccharomyces cerevisiae solution of 0.05, 0.10, 0.15 and 0.20%. The pomegranate wine was preserved at 14°C in dark bottle for different durations of 2, 4, 6, 8 weeks for secondary fermentation. Results indicated that 0.25% pectinase for 45 minutes was sufficient for juice extraction, 0.15% Sacchromyces cerevisiae solution for the main fermentation at 30±2°C and 6 weeks of aging in dark bottle at 14°C was appropriate to achieve a mild pomegranate wine. Fermentation by Saccharomyces cerevisiae and aging of wine resulted in changes of native substances into secondary metabolites influencing the sensory attributes of pomegranate wine.

Energetic Retrofit Strategies for Traditional Sicilian Wine Cellars: A Case Study

Sicily is characterized by rural buildings, Palmenti, destined to wine production, which are scattered along the countryside and part of the local historical heritage. There are different types of rural buildings, but all have in common the use of ancient and well-established bioclimatic techniques for wine conservation and aging. Most of them were built with the double function of living space for the owner and productive spaces for all the activities correlated to the cultivations. Indeed, many rural houses, destined to the wine production, are characterized by wineries and wine cellars (the first for the wine production, the second to store the wine for the aging process). The growing production of high-quality Sicilian wines, very appreciated all over the world, leads to upgrade the ancient Palmenti to seek optimal hygrothermal conditions and, therefore, to guarantee high performance of the produced and stored wines. The purpose of this study is to investigate how the retrofit measures taken to comply with the energy regulations could affect the thermal behavior of a wine cellar constructed with consolidated bioclimatic technics. The results show the importance of not insulating the solid ground floor for maintaining suitable temperatures for the fermentation and aging of wine. This study can be useful for future analysis when comparing the optimal hygrothermal conditions of wine cellars located in homogeneous viticultural areas (with same climate, geology, soil, physical features, and height) in other parts of the world.

Purification and characterization of Saccharomyces eubayanus killer toxin: Biocontrol effectiveness against wine spoilage yeasts

Microbiological contamination by spoilage yeasts species are frequent during winemaking, and biological control using antagonistic yeasts is considered a more beneficial alternative to conventional synthetic antimicrobials. Saccharomyces eubayanus killer toxin (SeKT) was produced and purified in a synthetic optimized medium. Purification procedure allowed the identification of SeKT as protein with an apparent molecular mass of 70 kDa and activity at physicochemical conditions suitable for winemaking process. Purified SeKT reduced the levels of volatile phenols produced by the spoilage yeasts Brettanomyces bruxellensis, Pichia membranifaciens, Meyerozyma guilliermondii and Pichia manshurica in wine-like medium. The putative mode of action of SeKT on sensitive yeast strains comprises cell wall disruption through β-glucanase and chitinase activities as well as necrotic and apoptotic death in a toxin dose dependent manner. Thus, SeKT appears to be a promising biocontrol agent against spoilage yeasts during wine aging and storing.

Volatile composition of oak wood from different customised oxygenation wine barrels: Effect on red wine

The compounds that the wood releases to the wine and the oxygen transmission rate (OTR) of the barrel define the final wine. The new possibility of choosing the OTR of the barrel allows the winemaker to globally control the ageing process. The aim of this work was to study the volatile composition of woods classified according to their OTR, which are used to build barrels for wine ageing. The results showed that volatile composition differs depending on wood OTR and the temperature reached during toasting. On the toasted side of the stave in contact with the wine, low OTR wood had a statistically higher content in furan compounds (5-hydroxymethylfurfural, furfural and 5-methylfurfural), acetovanillone and phenolic aldehydes (vanillin and syringaldehyde), while 4-ethylguaiacol and trans-β-methyl-γ-octalactone were significantly higher in staves with a high OTR. The same red wine aged first for three months in high and low oxygenation barrels presents different characteristics.

Study of the role of oxygen in the evolution of red wine colour under different ageing conditions in barrels and bottles

Wine ageing in barrels is conditioned, among other factors, by the amount of oxygen received during this process, which thus impacts its final properties. The aim of this study was to evaluate the effect of oxygen on wine colour during ageing in barrels and bottles during different times. The use of barrels with different and known rates of oxygenation allows the effect of different oxygenation conditions throughout the process in barrels and its later evolution in bottles. A simulation process of ageing in bottles was used to study the impact of bottling in wines after differing ageing periods in barrels. The study of winés oxygen consumption capacity has been tied to colour modifications during ageing in barrels and bottles. Wines aged in barrels with a high oxygenation rate showed greater avidity to consume oxygen taking less time to consume that available, which is reflected in a greater increase in colour intensity.

Influence of Different Modalities of Grape Withering on Volatile Compounds of Young and Aged Corvina Wines.

Withering is a practice traditionally used in various regions to produce sweet or dry wines. During withering there is an increase in sugar content but also a modification in volatile compound profiles. Controlling metabolic changes through the dehydration process to obtain wines with desired characteristics is therefore a challenging opportunity. The effects of two different withering technologies, post-harvest or on-vine with blocked sap vessel flow, on the volatile profile of young and aged Corvina red wines was investigated. The results showed that modulation of wine aroma due to the withering process is associated with fermentative metabolites, such as esters, higher alcohols, and acids, as well as grape-related compounds such as C6 alcohols, terpenes and norisoprenoids. Significant differences were also found by comparing the two withering techniques. Post-harvest in a traditional “fruttaio” warehouse wines showed higher content of ethyl acetate, ethyl butanoate, β-citronellol and 3-oxo-α-ionol, whereas post-harvest withering on-vine increased β-damascenone in wines. The type of withering technique has an influence on the evolution of some aroma compounds during the aging of wine, among them linalool, (E)-1-(2,3,6-trimethylphenyl)buta-1,3-diene (TPB), n-hexyl acetate, ethyl acetate, ethyl 3-methylbutanoate, 3-oxo-α-ionol and β-damascenone.

Age-dependent characterization of volatile organic compounds and age discrimination in Chinese rice wine using an untargeted GC/MS-based metabolomic approach

An untargeted gas chromatography/mass spectrometry (GC/MS)-based metabolomics by XCMS-Online software combined with partial least squares regression (PLSR) was applied to characterize volatile organic compounds (VOCs) during Chinese rice wine aging and discriminate ages for the first time. Finally, seven different ages between 0 and 15 years were well discriminated by PLSR. Total 104 feature groups were isolated from all optimized candidate peaks, and 94 VOCs (including unknowns) were preliminarily identified as aging markers. Therein, alcohols, sulfides, phenols and their derivatives, small esters and acids exhibited significantly better discrimination of short-aged rice wines. Correspondingly, furans, aromatics, aldehydes, ketones, most esters and acids, discriminated the long-aged samples better. Meanwhile, the potential origins of certain VOCs were also proposed for further research. Overall, this untargeted GC/MS-based metabolomics coupled with PLSR was a feasible tool for a rapidly and globally age-dependent characterization of volatile metabolomic signals in Chinese rice wine and thus for age discrimination.

Does barrel size influence white wine aging quality?

White wine is increasingly aged in oak barrels to enhance its stability, aromatic complexity and organoleptic properties. Thus, this research aimed to highlight chemical and sensory differences in Sauvignon Blanc wines linked to barrel size. Oenological parameters, color, total phenolics and fruity aroma were not generally impacted by barrel size. Meanwhile, the smaller the barrel, the higher the extraction of oak woody volatiles. From an organoleptic point of view, Sauvignon Blanc varietal aromas and typicity seemed to be better preserved by 500 L barrels.