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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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Keywords

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

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IVAS 2022 | IVES Conference Series

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Deconstructing the soil component of terroir: from controversy to consensus

Wine terroir describes the collectively recognized relation between a geographical area and the distinctive organoleptic characteristics of the wines produced in it. The overriding objective in terroir studies is therefore to provide scientific proof relating the properties of terroir components to wine quality and typicity. In scientific circles, the role of climate (macro-, meso- and micro-) on grape and wine characteristics is well documented and accepted as the most critical. Moreover, there has been increasing interest in recent years about new elements with possible importance in shaping wine terroir like berry/leaf/soil microbiology or even aromatic plants in proximity to the vineyard conferring flavors to the grapes. However, the actual effect of these factors is also dependent on complex interactions with plant material (variety/clone, rootstock, vine age) and with human factors.
The contribution of soil, although a fundamental component of terroir and extremely popular among wine enthusiasts, remains a much-debated issue among researchers. The role of geology is probably the one mostly associated by consumers with the notion of terroir with different parent rocks considered to give birth to different wine styles. However, the relationship between wine properties and the underlying parent material raises a lot of controversy especially regarding the actual existence of rock-derived flavors in the wine (e.g. minerality). As far as the actual soil properties are concerned, the effect of soil physical properties is generally regarded as the most significant (e.g sandy soils being associated with lighter wines while those on clay with colored and tannic ones) mostly through control of water availability which ultimately modifies berry ripening conditions either directly by triggering biosynthetic pathways, or indirectly by altering vigor and yield components. The role of soil chemistry seems to be weakly associated to wine sensory characteristic, although N, K, S and Ca, but also soil pH, are often considered important in the overall soil effect.
Recently, in the light of evidence provided by precision agriculture studies reporting a high variability of vineyard soils, the spatial scale should also be taken into consideration in the evaluation of the soil effects on wines. While it is accepted that soil effects become more significant than climate on a local level, it is not clear whether these micro-variations of vineyard soils are determining in the terroir effect. Moreover, as terroir is not a set of only natural factors, the magnitude of the contribution of human-related factors (irrigation, fertilization, soil management) to the soil effect still remains ambiguous. Lastly, a major shortcoming of the majority of works about soil effects on wine characteristics is the absence of connection with actual vine physiological processes since all soil effects on grape and wine chemistry and sensorial properties are ultimately mediated through vine responses.
This article attempts to breakdown the main soil attributes involved in the terroir effect to suggest an improved understanding about soil’s true contribution to wine sensory characteristics. It is proposed that soil parameters per se are not as significant determining factors in the terroir effect but rather their mutual interactions as well as with other natural and human factors included in the terroir concept. Consequently, similarly to bioclimatic indices, composite soil indices (i.e. soil depth, water holding capacity, fertility, temperature etc), incorporating multiple soil parameters, might provide a more accurate and quantifiable means to assess the relative weight of the soil component in the terroir effect.

Climate change impacts on Douro Region viticulture and adaptation measures

Climate has a significant impact in the success of any agricultural system, with a direct influence on the crops suitability to a given region, interfering on yield and quality and also with the economic sustainability of the productive activity. In the Douro Demarcated Region (RDD), as in most regions of the Mediterranean climate, the scarce precipitation (33% has less than 600 mm per year), and your high variability, associated with high rates of evapotranspiration during the summer, is usually one of the fundamental factors that limit the grapevine development, as well as the production and quality of the harvest. Thus, facing the scenario in temperature changes for the next decades (1.5-2.5°C) and confirming the predictions of precipitation decreases and/or great variability in the occurrence of heat waves and intense rainfall, the consequences for slope stability in mountain viticulture and sustainability of all operations involved, are risks to be taken into account. In this way, a deepest and sustained knowledge regarding the adaptation measures to adverse environmental conditions is of a crucial importance, enabling a more efficient adaptation of plant growth conditions and the optimization of production and quality of the grapevines. The development of this work, carried out in two commercial vineyards, one located in Soutelo do Douro, São João da Pesqueira, Cima Corgo sub-region, and another located in Numão, Vila Nova de Foz Côa, Douro Superior sub-region, it seeks to establish a relationship between climatic elements and physiological, productive and qualitative parameters, as well as to evaluate the effectiveness of adaptation measures, including different types of deficit irrigation (2002-2019) and the application of shading nets (2019-2020) in the physiological, viticultural and oenological behavior in the Touriga Nacional and Moscatel Galego Branco varieties, respectively. The results showed that the application of deficit irrigation allowed to significantly reduce the impact of the adverse weather conditions at key moments in the development of the grapevine, particularly in the period immediately before veráison and maturation, reducing the negative effects on the physiological processes and productivity, without compromise the must quality parameters. On the other hand, the application of shading nets significantly reduced de leaves temperature, allowing to increase the water potential, stomatal conductance and photosynthetic rate of grapes, which was reflected in the yield increase in the 2nd year of the study. For the maturation indicators, higher levels of total acidity, malic acid and assimilable nitrogen were obtained. The last measure presents a huge potential, being essential to carry out more years of trials to obtain stronger conclusions in terms of production parameters, but also in characteristics as important as the grape ripening components and the organoleptic characteristics of wines.

Legacy of land-cover changes on soil erosion and microbiology in Burgundian vineyards

Soils in vineyards are recognized as complex agrosystems whose characteristics reflect complex interactions between natural factors (lithology, climate, slope, biodiversity) and human activities. To date, most of the unknown lies in an incomplete understanding of soil ecosystems, and specifically in the microbial biodiversity even though soil microbiota is involved in many key functions, such as nutrient cycling and carbon sequestration. Soil biological properties are indicative of soil quality. Therefore, understanding how soil communities are related to soil ecosystem functioning is becoming an essential issue for soil strategy conservation. Here, we propose to assess the importance of land-cover history on the present-day microbiological and physico-chemical properties. The studied area was selected in the Burgundian vineyards (Pernand-Vergelesses, Burgundy, France) where land occupation has been reconstructed over the last 40 years. Soil samples were collected in five areas reflecting various land cover history (forest, vineyards, shifting from forest to vineyards). For each area, physico-chemical parameters (pH, C, N, P, grain size) were measured and DNA was extracted to characterize the abundance and diversity of microbial communities. The obtained results show significant differences in the five areas suggesting that present-day microbial molecular biomass and bacterial taxonomic is partly inherited from past land occupation. Over longer period of time, such study of land-uses legacies may help to better assess ecosystem recovery and the impact of management practices for a better soil quality and vineyards sustainability.

Low-cost sensors as a support tool to monitor soil-plant heat exchanges in a Mediterranean vineyard

Mediterranean viticulture is increasingly exposed to more frequent extreme conditions such as heat waves. These extreme events co-occur with low soil water content, high air vapor pressure deficit and high solar radiant energy fluxes and result in leaf and berry sunburn, lower yield, and berry quality, which is a major constraint for the sustainability of the sector. Grape growers must find ways to proper and effectively manage heat waves and extreme canopy and berry temperatures. Irrigation to keep soil moisture levels and enable adequate plant turgor, and convective and evaporative cooling emerged as a key tool to overcome this major challenge. The effects of irrigation on soil and plant water status are easily quantifiable but the impact of irrigation on soil and canopy temperature and on heat convection from soil to cluster zone remain less characterized. Therefore, a more detailed quantification of vineyard heat fluxes is highly relevant to better understand and implement strategies to limit the effects of extreme weather events on grapevine leaf and berry physiology and vineyards performance. Low-cost sensor technologies emerge as an opportunity to improve monitoring and support decision making in viticulture. However, validation of low-cost sensors is mandatory for practical applicability. A two-year study was carried in a vineyard in Alentejo, south of Portugal, using low-cost thermal cameras (FLIR One, 80×60 pixels and FLIR C5, 160×120 pixels, 8-14 µm, FLIR systems, USA) and pocket thermohygrometers (Extech RHT30, EXTECH instruments, USA) to monitor grapevine and soil temperatures. Preliminary results show that low-cost cameras can detect severe water stress and support the evaluation of vertical canopy temperature variability, providing information on soil surface temperature. All these thermal parameters can be relevant for soil and crop management and be used in decision support systems.

Upscaling the integrated terroir zoning through digital soil mapping: a case study in the Designation of Origin Campo de Borja

homogeneous zones by intersecting several partial zonings of major factors that influence vineyard growth. Each of them follows specific process from their corresponding disciplines. Soil zoning specifically refers to a Soil Resource Inventory map that has traditionally been generated by conventional soil mapping methods. These methods have shortcomings in reaching fine cartographic and categorical details and involve significant expenses, which undermines their applicability. A new framework named Digital Soil Mapping has introduced quantitative models by statistical techniques to establish soil-landscape relationships and is able to provide intensive scale cartography.

In the present study, a microzoning at 1:10.000 scale is generated from an initial zoning, where the conventional soil map with polytaxic map units is replaced by a new one from digital techniques that disaggregates them. The comparison between the zonings considers a quantitative evaluation of capability for each Homogeneous Terroir Unit by means of the Viticultural Quality Index and its categorization based on its distribution by map. The spatial intersection of both maps gives rise to a confusion matrix in which the flows of class variations after the substitution are assessed.

The results show a five-fold increase in the number of Homogeneous Terroir Units identified and a larger differentiation among them, evidenced by a wider range in the capability index distribution. Both elements are accompanied by an increase in the detection of areas of higher potential within previously undervalued uniform zones.These features are a direct effect of the improvements brought by Digital Soil Mapping techniques and would verify the advantages of their implementation in the Integrated Terroir zoning. Eventually, such new highly detailed terroir units would benefit precision viticulture and sustainable management practices.

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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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Effect of one-year cover crop and arbuscular mycorrhiza inocululation in the microbial soil community of a vineyard

The microbial composition of the soil is an important factor to consider in viticulture, since its influence on the “terroir” and on the organoleptic properties of the wine have been demonstrated. Different agronomic techniques have the potential to modify the composition and functionality of the soil microbial community. Maintaining green covers is known to increase soil microbial diversity. The direct application of inoculum of beneficial microorganisms to the soil has also been used to increase their abundance. However, the environmental conditions of each site seem to have a determining weight in the result of these practices. In this study, we compared the effect on the microbial community of a cover crop with legumes in autumn and the inoculation of grapevines with commercial inoculum bases on Rhizophagus irregularis and Funeliformis mosseae in the previous spring. The study has been carried out in a vineyard in Binissalem, Mallorca, Spain. After applying the treatments, we will analyze the soil microbial communities using the data obtained from Illumina amplification of soil DNA from the 16S and ITS regions to analyze bacteria and fungi community, respectively. In addition, we will record the physicochemical characteristics of the soil at each sampling point. The result showed that agronomic management, in the short term, has less influence than soil characteristics on the composition of the soil microbiome. With these results, we can conclude that in a vineyard, agricultural techniques should focus on improving the characteristics of the soil to improve the biodiversity of the soil microbiota.

Upscaling the integrated terroir zoning through digital soil mapping: a case study in the Designation of Origin Campo de Borja

homogeneous zones by intersecting several partial zonings of major factors that influence vineyard growth. Each of them follows specific process from their corresponding disciplines. Soil zoning specifically refers to a Soil Resource Inventory map that has traditionally been generated by conventional soil mapping methods. These methods have shortcomings in reaching fine cartographic and categorical details and involve significant expenses, which undermines their applicability. A new framework named Digital Soil Mapping has introduced quantitative models by statistical techniques to establish soil-landscape relationships and is able to provide intensive scale cartography.

In the present study, a microzoning at 1:10.000 scale is generated from an initial zoning, where the conventional soil map with polytaxic map units is replaced by a new one from digital techniques that disaggregates them. The comparison between the zonings considers a quantitative evaluation of capability for each Homogeneous Terroir Unit by means of the Viticultural Quality Index and its categorization based on its distribution by map. The spatial intersection of both maps gives rise to a confusion matrix in which the flows of class variations after the substitution are assessed.

The results show a five-fold increase in the number of Homogeneous Terroir Units identified and a larger differentiation among them, evidenced by a wider range in the capability index distribution. Both elements are accompanied by an increase in the detection of areas of higher potential within previously undervalued uniform zones.These features are a direct effect of the improvements brought by Digital Soil Mapping techniques and would verify the advantages of their implementation in the Integrated Terroir zoning. Eventually, such new highly detailed terroir units would benefit precision viticulture and sustainable management practices.

Leaf vine content in nutrients and trace elements in La Mancha (Spain) soils: influence of the rootstock

The use of rootstock of American origin has been the classic method of fighting against Phylloxera for more than 100 years. For this reason, it is interesting to establish if different rootstock modifies nutrient composition as well as trace elements content that could be important for determining the traceability of the vine products. A survey of four classic rootstocks (110-Richter, SO4, FERCAL and 1103-Paulsen) and four new ones (M1, M2, M3 and M4) provided by Agromillora Iberia. S.L.U., all of them grafted with the Tempranillo variety, has been carried out during 2019. The eight rootstocks were planted in pots of 500 cc, on three soils with very different characteristics from Castilla-La Mancha (Spain). In the month of July, the leaves were collected and dried in a forced air oven for seven days at 40ºC. Then, the samples were prepared for the analysis determination, carried out by X-Ray fluorescence spectrometry. The results obtained showed that in the case of content in mineral elements in leaf, separated by soil type, we can report the importance of few elements such as Si, Fe, Pb and, especially, Sr. The rootstock does not influence the composition of the vine leaf for the studied elements that are the most important in determining the geochemical footprint of the soil. The influence of the soil can be discriminated according to some elements such as Fe, Pb, Si and, especially, Sr.

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.

Delaying irrigation initiation linearly reduces yield with little impact on maturity in Pinot noir

When to initiate irrigation is a critical annual management decision that has cascading effects on grapevine productivity and wine quality in the context of climate change. A multi-site trial was begun in 2021 to optimize irrigation initiation timing using midday stem water potential (ψstem) thresholds characterized as departures from non-stressed baseline ψstemvalues (Δψstem). Plant material, vine and row spacing, and trellising systems were concomitant among sites, while vine age, soil type, and pruning systems varied. Five target Δψstem thresholds were arranged in an RCBD and replicated eight times at each site: 0.2, 0.4, 0.6, 0.8, and 1.0 MPa (T1, T2, T3, T4, and T5, respectively). When thresholds were reached, plots were irrigated weekly at 70% ETc. Yield components and berry composition were quantified at harvest. To better generalize inferences across sites, data were analyzed by ANOVA using a mixed model including site as a random factor. Across sites, irrigation was initiated at Δψstem = 0.24, 0.50, 0.65, 0.93, and 0.98 MPa for T1, T2, T3, T4, and T5, respectively. Consistent significant negative linear trends were found for several key yield and berry composition variables. Yield decreased by 12.9, 15.9, 19.5, and 27.4% for T2, T3, T4, and T5, respectively, compared to T1 (p < 0.0001) across sites that were driven by similarly linear reductions in berry weight (p < 0.0001). Comparatively, berry composition varied little among treatments. Juice total soluble solids decreased linearly from T1 to T5 – though only ranged 0.9 Brix (p = 0.012). Because producers are paid by the ton, and contracts simply stipulate a target maturity level, first-year results suggest that there is no economic incentive to induce moderate water deficits before irrigation initiation, regardless of vineyard site. Subsequent years will further elucidate the carryover effects of delaying irrigation initiation on productivity over the long term.