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IVES 9 IVES Conference Series 9 IVAS 9 IVAS 2022 9 Optimization and validation of a fully automated HS-SPME method for determination of VCCs and its application in wines submitted to accelerated ageing

Optimization and validation of a fully automated HS-SPME method for determination of VCCs and its application in wines submitted to accelerated ageing

Abstract

Wine aroma is a complex gaseous mixture composed of various compounds; some of these molecules derive directly from the grapes while most of them are released and synthetized during fermentation or are due to ageing reactions. Among the latter class of compounds, carbonyls are the principal products of oxidation reactions which take place during the storing time. Volatile carbonyl compounds (VCCs) are related to aromatic nuances of vanilla, caramel, butter, honey, potato, orange, lemon, violets, cider and plum, which are pleasant scents characteristics of oxidized wines. However, apart from cases where it is a deliberate process, oxidation is commonly undesired and the presence of a relevant content of carbonyls is related to aroma defects. Because of that, monitoring the concentration of VCCs could be added as a quality control for the evaluation of a complete fermentation, correct winemaking style, and proper bottling and storage. In this research an HS-SPME method1 was optimized and validated with the aim to be used as a tool to achieve this goal. The use of a solvent-free extraction allowed to maximize the coherence to the Green Analytical Chemistry principles with a simultaneous achievement in performance, reliability and robustness. In this method, all sample preparation steps were automated using the autosampler minimizing the human time consumption to enhance the scalability to routine analysis. As many as 46 VCCs (mainly linear aldehydes, Strecker aldehydes, unsaturated aldehydes, ketones, and many other) were the analytes under investigation. All compounds showed a good linearity spanning from approximately 0.1 to 100 µg/L (R2>0.99). Intra-day and 5 days inter-days repeatability showed an RSD

DOI:

Publication date: June 23, 2022

Issue: IVAS 2022

Type: Article

Authors

Piergiovanni Maurizio1, Carlin Silvia2, Lotti Cesare2, Vhrovsek Urska2 and Mattivi Fulvio1,2

1Center Agriculture Food Environment (C3A), University of Trento, via Edmund Mach 1, San Michele all’Adige (TN) Italy
2Center Research and Innovation, Edmund Mach Foundation, Italy3Affiliation of the third 

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Carbonyls, oxidation, accelerated ageing, HS-SPME, quality control

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Rootstock regulation of scion phenotypes: the relationship between rootstock parentage and petiole mineral concentration

Grapevine is grown as a graft since the end of the 19th century. Rootstocks not only provide tolerance to Phylloxera but also ensure the supply of water and mineral nutrients to the scion. Rootstocks are an important mean of adaptation to environmental conditions, because the scion controls the typical features of the grapes and wine. However, among the large diversity of rootstocks worldwide, few of them are commercially used in the vineyard. The aim of this study was to investigate the extent to which rootstocks modify the mineral composition of the petioles of the scion. Vitis vinifera cvs. Cabernet-Sauvignon, Pinot noir, Syrah and Ugni blanc were grafted onto 55 different rootstock genotypes and planted in a vineyard as three replicates of 5 vines. Petioles were collected in the cluster zone with 6 replicates per combination. Petiolar concentrations of 13 mineral elements (N, P, K, S, Mg, Ca, Na, B, Zn, Mn, Fe, Cu, Al) at veraison were determined. Scion, rootstock and the interaction explained the same proportion of the phenotypic variance for most mineral elements. Rootstock genotype showed a significant influence on the petiole mineral element composition. Rootstock effect explained from 7 % for Cu to 25 % for S of the variance. The difference of rootstock conferred mineral status is discussed in relation to vigor and fertility. Rootstocks were also genotyped with 23 microsatellite markers. Data were analysed according to genetic groups in order to determine whether the petiole mineral composition could be related to the genetic parentage of the rootstock. Thanks to a highly powerful design, it is the first time that such a large panel of rootstocks grafted with 4 scions has been studied. These results give the opportunity to better characterize the rootstocks and to enlarge the diversity used in the vineyard.

Influence of climatic conditions on grape composition of Tempranillo in La Mancha DO (Spain)

The aim of this work was to analyze the variability in grape composition of the Tempranillo cultivar related to climatic conditions, in La Mancha Designation of Origin. Grape composition (sugar content, total acidity, pH, malic acid, and total and extractable anthocyanins) recorded during ripening, were analysed for the period 2000-2019. The weather conditions at daily time scale, recorded during the same period, were also evaluated. The relationships between grape parameters with climatic variables related to temperature and to water deficits, referring different periods between phenological events along the growing cycle, were evaluated using regression analysis. High variability in grape composition was observed in the period analysed. Total acidity varied between 3.7 and 7.3 gL-1 while malic acid varied between 1.2 and 4 gL-1. The extractable anthocyanins ranged between 526 and 972 mgL-1, and total anthocyanins ranged between 922 and 1388 mgL-1, being the lowest values recorded in the hottest year (2017). Total acidity decreased 0.77 gL-1 for an increase of 100 GDD, while malic acid decrease in 0.42 gL-1 for the same GDD increase, being the period between veraison and harvest the one that seemed to have higher influence on acidity. In addition, it was confirmed that increasing water deficits decreased acidity. Total and extractable anthocyanins increased in about 210 and 105 mgL-1, respectively, with an increase of 100 GDD from veraison to harvest, and the increase in water deficits favour the increase of anthocyanins, both total and extractable anthocyanins. Total and extractable anthocyanins concentration increased in 35 and 22 mgL-1 per an increase of 10 mm in the water deficit. These results can be of interest to understand the potential changes that grapes composition may suffer under future warmer climates.

Mesoclimate impact on Tannat in the Atlantic terroir of Uruguay

The study of climate is relevant as an element conditioning the typicity of a product, its quality and sustainability over the years. The grapevine development and growth and the final grape and wine composition are closely related to temperature, while climate components vary at mesoscale according to topography and/or proximity to large bodies of water. The objective of this work is to assess the mesoclimate of the Atlantic region of Uruguay and to determine the effect of topography and the ocean on temperature and consequently on Tannat grapevine behavior.

Grapevine sugar concentration model in the Douro Superior, Portugal

Increasingly warm and dry climate conditions are challenging the viticulture and winemaking sector. Digital technologies and crop modelling bear the promise to provide practical answers to those challenges. As viticultural activities strongly depend on harvest date, its early prediction is particularly important, since the success of winemaking practices largely depends upon this key event, which should be based on an accurate and advanced plan of the annual cycle. Herein, we demonstrate the creation of modelling tools to assess grape ripeness, through sugar concentration monitoring. The study area, the Portuguese Côa valley wine region, represents an important terroir in the “Douro Superior” subregion. Two varieties (cv. Touriga Nacional and Touriga Franca) grown in five locations across the Côa Region were considered. Sugar accumulation in grapes, with concentrations between 170 and 230 g l-1, was used from 2014 to 2020 as an indicator of technological maturity conditioned by meteorological factors. The climatic time series were retrieved from the EU Copernicus Service, while sugar data were collected by a non-profit organization, ADVID, and by Sogrape, a leading wine company. The software for calibrating and validating this model framework was the Phenology Modeling Platform (PMP), version 5.5, using Sigmoid and growing degree-day (GDD) models for predictions. The performance was assessed through two metrics: Roots Mean Square Error (RMSE) and efficiency coefficient (EFF), while validation was undertaken using leave-one-out cross-validation. Our findings demonstrate that sugar content is mainly dependent on temperature and air humidity. The models achieved a performance of 0.65

The rootstock, the neglected player in the scion transpiration even during the night

Water is the main limiting factor for yield in viticulture. Improving drought adaptation in viticulture will be an increasingly important issue under climate change. Genetic variability of water deficit responses in grapevine partly results from the rootstocks, making them an attractive and relevant mean to achieve adaptation without changing the scion genotype. The objective of this work was to characterize the rootstock effect on the diurnal regulation of scion transpiration. A large panel of 55 commercial genotypes were grafted onto Cabernet Sauvignon. Three biological repetitions per genotype were analyzed. Potted plants were phenotyped on a greenhouse balance platform capable of assessing real-time water use and maintaining a targeted water deficit intensity. After a 10 days well-watered baseline period, an increasing water deficit was applied for 10 days, followed by a stable water deficit stress for 7 days. Pruning weight, root and aerial dry weight and transpiration were recorded and the experiment was repeated during two years. Transpiration efficiency (ratio between aerial biomass and transpiration) was calculated and δ13C was measured in leaves for the baseline and stable water deficit periods. A large genetic variability was observed within the panel. The rootstock had a significant impact on nocturnal transpiration which was also strongly and positively correlated with maximum daytime transpiration. The correlations with growth and water use efficiency related traits will be discussed. Transpiration data were also related with VPD and soil water content demonstrating the influence of environmental conditions on transpiration. These results highlighted the role of the rootstock in modulating water deficit responses and give insights for rootstock breeding programs aimed at identifying drought tolerant rootstocks. It was also helpful to better define the mechanisms on which the drought tolerance in grapevine rootstocks is based on.

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IVES 9 IVES Conference Series 9 IVAS 9 IVAS 2022 9 Optimization and validation of a fully automated HS-SPME method for determination of VCCs and its application in wines submitted to accelerated ageing

Optimization and validation of a fully automated HS-SPME method for determination of VCCs and its application in wines submitted to accelerated ageing

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Publication date: June 23, 2022

Issue: IVAS 2022

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Copper contamination in vineyard soils of Bordeaux: spatial risk assessment for the replanting of vines and crops

Copper (Cu) is widely and historically used in viticulture as a fungicide against mildew. Cu has a strong affinity for soil organic matter and accumulates in topsoil horizons. Thus, Cu may negatively affect soil organisms and plants, consequently reducing soil fertility and productivity. The Bordeaux vineyards have the largest vineyard surfaces (26%) within French controlled appellation and a great proportion of French wine production (around 5 million hl per year). Considering the local context of vineyard surfaces decreasing (vine uprooting) and possible new crop plantation, the issue of Cu potential toxicity rises. Therefore, the aims of this work are firstly to evaluate the Cu contamination in vineyard soils of Bordeaux, secondly to produce a risk assessment map for new vine or crop plantation. We used soil analyses from several local studies to build a database with 4496 soil horizon samples. The database was enhanced by means of pedotransfer functions in order to estimate the bioaccessible (EDTA-extractable) Cu in soils of samples without measurements. From this database, 1797 georeferenced samples with CuEDTA concentrations in the topsoil (0-50 cm depth) were used for kriging interpolation in order to produce the spatial distribution map of CuEDTA in vineyard soils. Then, the spatial distribution of Cu was crossed with vine uprooting surfaces and municipality boundaries. CuEDTAconcentrations ranged from 0.52 to 459 mg/kg and showed clear anomalies. Our results from spatial analysis showed that almost 50% of vineyard soil surfaces have CuEDTA concentrations higher than 30 mg/kg (moderate risk for new plantation) and 20% with concentrations higher than 50 mg/kg (high risk for new plantation). A decision-support map based on municipalities was realised to provide a simple tool to stakeholders concerned by land use management.

Mobile device to induce heat-stress on grapevine berries

Studying heat stress response of grapevine berries in the field often relies on weather conditions during the growing season. We constructed a mobile heating device, able to induce controlled heat stress on grapes in vineyards. The heater consisted of six 150 W infrared lamps mounted in a profile frame. Heating power of the lamps could be controlled individually by a control unit consisting of a single board computer and six temperature sensors to reach a pre-set temperature. The heat energy applied to individual berries within a cluster decreases by the squared distance to the heat source, enabling the establishment of temperature profiles within individual clusters. These profiles can be measured by infrared thermography once a steady state has been reached. Radiant flux density received by a berry depending on the distance was calculated based on a view factor and measured lamp surface temperature and resulted to 665 Wm-2 at 7cm. Infrared thermography of the fruit surface was in good agreement with measurements conducted with a thermocouple inserted at epidermis level. In combination with infrared thermography, the presented device offers possibilities for a wide range of applications like phenotyping for heat tolerance in the field to proceed in the understanding of the complex response of plants to heat stress. Sunburn necrosis symptoms were artificially induced with the aid of the device for cv. Bacchus and cv. Sylvaner in the 2020 and 2021 growing season. Threshold temperatures for sunburn induction (LT5030min) were derived from temperature data of single berries and visual sunburn assessment, applying logistic regression. A comparison of threshold temperatures for the occurrence of sunburn necrosis confirmed the higher susceptibility of cv. Bacchus. The lower susceptibility of cv. Sylvaner did not seem to be related to its phenolic composition, rendering a thermoprotective role of berry phenolic compounds unlikely.

Modulation of berry composition by different vineyard management practices

High concentration of sugars in grapes and alcohol in wines is one of the consequences of climate change on viticulture production in several wine-growing regions. In order to investigate the possibilities of adaptation of vineyard management practices aimed to reduce the accumulation of sugar during the maturation phase without reducing the accumulation of anthocyanins in grapes, a study with severe shoot trimming, shoot thinning, cluster thinning and date of harvest was conducted on Merlot variety in Istria region (Croatia), under the Mediterranean climate. Four factors which may affect grape maturation and its composition at harvest were investigated in a two-years experiment; severe shoot trimming applied at veraison when >80% of berries changed colour (in comparison to untreated control), shoot thinning (0 and 30%), cluster thinning (0 and 30%), and the date of harvest (early and standard harvest dates). Shoot thinning had no significant impact on berry composition, despite the obtained reduction in yield per vine. Lower Brix in grapes were obtained with earlier harvest date and if no cluster thinning was applied, although at the same time a reduction in the concentration of anthocyanins in berries was observed in these treatments. On the other hand, if severe shoot trimming was applied when >80% of berries changed colour, a reduction of Brix was obtained without a negative impact on berry anthocyanins concentration. We conclude that in cases when undesirably high sugar concentrations at harvest are expected, severe shoot trimming at 80% veraison may effectively be used in order to obtain moderate sugar concentration in berries together with the adequate phenolic composition.

How can historical cultivars mitigate the effects of climate change?

IFV, INRAe and the national network “Partenaires de la Sélection Vigne” representing 37 organizations from the different wine regions, have been working increasingly closely over the last 2 decades towards the preservation of the French varietal patrimony. There are approximately 600 patrimonial varieties according to INRAe and SupAgro Montpellier experts, including ancient cultivars (400) and intravarietal crossbreeds obtained since the 19th century. In the context of a drastic reduction in such varieties from the mid 1980’s in favor of mainstream varieties, it was essential to carry out an inventory of old vines and vineyards. INRAe Vassal collection plays a key role here as it holds the largest diversity available, along with a rich bibliography and herbariums, offering us the opportunity to document and double check the identity of a cultivar, consolidating the expertise of ampelographers. The work is carried out in several stages, from verifying the existence of a variety in a small region, through to rehabilitation. During this session, the authors present the process that leads to the official registration of a variety. After this, IFV selection center takes over to initiate the process of selection and propagation. A specific focus within regions such as the Alps, Champagne and the South-West will provide details of the full procedure. Bia, Bouysselet, Chardonnay rose, Mecle and the aptly named Tardif, are some of the cultivars that have followed this procedure. Furthermore, a recent regulation established by INAO on “varieties of interest for adaptation purposes” might boost uptake by growers. Since 2006, 36 historical cultivars have been registered. Most of these have been neglected in the past due to late maturity, lack of sugar and high titratable acidity at harvest time. Such characteristics are today considered as positive qualities, not only in mitigation of the effects of climate change, but also as an opportunity for restoring diversity…

How distinctive are single vineyard Gewürztraminer musts and wines from Alto Adige (Italy) based on untargeted analysis, sensory profiling, and chemometric elaboration?

Vitis vinifera L. ‘Gewürztraminer’ is a historical grape variety of Alto Adige (Südtirol), Italy, which is widely grown in the area of Tramin an der Weinstraße, but is also grown globally. It produces highly aromatic wines that are strongly influenced by the terroir of the vineyard sites where they are grown. This study looked at musts and young wines from ‘Gewürztraminer’ grapes harvested in seven distinct vineyards near Tramin and then processed at Cantina di Termeno, minimizing winemaking protocol variability. Samples were profiled using bidimensional gas chromatography–time-of-flight mass spectrometry, liquid chromatography coupled to electrochemical detection, and near-IR spectrometry. The data were subjected to Principle Component Analysis and Hierarchical Clustering Analysis. Sensory discriminant testing was undertaken using the sorting method with a semi-trained panel, and the data were processed using Multidimensional Scaling. Seven must/wine pairs could be distinguished based on their untargeted volatilome profiles and on sensory evaluation. As expected, there were greater differences in the volatile compounds between the wines than between the musts. The wines from vineyards 4 and 5 were nonetheless quite homogenous in terms of chemical and sensory analyses, as were the wines from vineyards 1 and 3. For the phenolic profile, differences were noted between the musts and wines of vineyards 2, 3, and 4, but the musts from vineyards 5 and 7 were similar. Sensory analysis showed the wines from vineyards 6 and 7 to be distinct from the rest. These results reinforce that the composition of ‘Gewürztraminer’ musts and wines is strongly determined by vineyard site, even in a small geographic area with high variability of the terroir (soil and microclimate), and that these differences are apparent in the flavours and aromas of the finished wines. Further confirmation would require a larger sample of wines, preferably from several vintages.