IVAS 2022 banner
IVES 9 IVES Conference Series 9 IVAS 9 IVAS 2022 9 Exploring and unravelling the complex toasted oak wood (Q. sp.) volatilome using GCxGC-TOFMS technique

Exploring and unravelling the complex toasted oak wood (Q. sp.) volatilome using GCxGC-TOFMS technique

Abstract

For coopers, toasting process is considered as a crucial step in barrel production where oak wood develops several specific aromatic nuances released to the wine during its maturation. Toasting is applying varying degrees of heat to a barrel over a specific amount of time. Today it is well known that as the temperature increases, thermal degradation of oak wood structure produces a huge range of chemical compounds. Indeed, many works were conducted to identify key aroma volatile compounds (e.g., whisky-lactone, furfural, maltol, eugenol, guaiacol, vanillin) using the traditional gas chromatography coupled with olfactometry and mass spectrometry (GC-O-MS).

Inspired by recent untargeted approaches in food “omics”, this work aims at expanding our knowledge on oak wood volatile composition by bi-dimensional comprehensive gas chromatography-time of flight mass spectrometry (GCxGC-TOFMS, BT4D, Leco).

In a first experiment, five toasting levels were selected and applied to Q. sessilis oak wood samples (control, 160 °C, 180 °C, 200 °C and 220 °C, 30 min, n=3). Organic extracts were prepared (dichloromethane, 50 g/L) and analysed by GCxGC-TOFMS on conventional column combination nonpolar/midpolar (DB-5ms/Rxi-17Sil). The separation was followed by a non-targeted approach for data processing. The resulting mass spectra (TIC) were de convoluted (ChromaTOF software) and compared to spectra from a database for tentative peak identification. It was necessary to restrict the number of processed peaks by applying some “filters” such as signal to noise (S/N > 50), linear retention index (LRI ± 30), mass spectra similarity (> 750) and repeatability level. Supervised multivariate and univariate statistical approaches were used to identify potential markers of toasting intensity. Thanks to R script, reproducible peaks number was reduced from about 15000 to 568. By comparing observed retention indices with those found in the literature, 77 of the identifications have been confirmed and associated with an increase in toasting intensity. Some of them were sensory active and well known in oak wood, such as guaiacol, creosol and isoeugenol. Others were identified for the first time in toasted oak wood such as 2-methylbenzofurane (burnt) and 2-hydroxy-2-cyclopenten-1-one (caramel).Additional results were also discussed on the capability of GCxGC-TOFMS to identify oak wood botanic origins (Q. robur, Q. alba

DOI:

Publication date: June 23, 2022

Issue: IVAS 2022

Type: Article

Authors

Courregelongue Marie1,², Albertin Warren1,³, Prida Andrei2 and Pons Alexandre1,²

¹UMR ŒNOLOGIE (OENO), ISVV, UMR 1366, Université de Bordeaux, INRAE, Bordeaux INP
²Tonnellerie Seguin Moreau, Merpins, France
³ENSCBP, Bordeaux INP, 33600, Pessac, France

Contact the author

Keywords

non-targeted analysis, GCxGC-TOFMS, oak wood, toasting process, volatile compounds

Tags

IVAS 2022 | IVES Conference Series

Citation

Related articles…

Modeling the suitability of Pinot Noir in Oregon’s Willamette Valley in a changing climate

Air temperature is the key driver of grapevine phenology and a significant environmental factor impacting yield and quality for a winegrape growing region. In this study the optimal downscaled CMIP5 ensemble for computing thegrowing season average temperature (GST) viticulture climate classification index was determined to spatially compute on a decadal basis predictions of the GST climate index and the grapevine sugar ripeness (GSR) model for Pinot Noir throughout the Willamette Valley (WV) American Viticultural Area (AVA). Forecasts for average temperature and a 220 g/L target sugar concentration level were computed using daily Localized Constructed Analogs (LOCA) downscaled CMIP5 historic and Representative Concentration Pathways (RCP) future climate projections of minimum and maximum daily temperature. We explore spatiotemporal trends of the GST climate classification index and Pinot Noir specific applications of the GSR phenology model for the WV AVA. Spatiotemporal computations of the GST climate index and Pinot Noir specific applications of the GSR model enable the opportunity to explore relationships between their computed values with one intent being to provide updated GST ranges that better align with current temperature-based modeling understanding of Pinot Noir grapevine phenology and the viticultural application of LOCA CMIP5 climate projections for the WV AVA. The Pinot Noir specific applications of the GSR model or the GST index with updated bounds indicate that the percent of the WV AVA area suitable for Pinot Noir production is currently at or near its peak value in the upper 80s to lower 90s of this century.

Using δ13C and hydroscapes as a tool for discriminating cultivar specific drought response

Measurement of carbon isotope discrimination in berry juice sugars at maturity (δ13C) provides an integrated assessment of water use efficiency (WUE) during the period of berry ripening, and when collected over multiple seasons can be used as an indication of drought stress response. Berry juice δ13C measurements were carried out on 48 different varieties planted in a common garden experiment in Bordeaux, France from 2014 through 2021 and were paired with midday and predawn leaf water potential measurements on the same vines in a subset of six varieties. The aim was to discriminate a large panel of varieties based on their stomatal behaviour and potentially identify hydraulic traits characterizing drought tolerance by comparing δ13C and hydroscapes (the visualisation of plant stomatal behaviour as a response to predawn water potential). Cluster analysis found that δ13C values are likely affected by the differing phenology of each variety, resulting in berry ripening of different varieties taking place under different stress conditions within the same year. We accounted for these phenological differences and found that cluster analysis based on specific δ13C metrics created a classification of varieties that corresponds well to our current empirical understanding of their relative drought tolerances. In addition, we analysed the water potential regulation of the subset of six varieties (using the hydroscape approach) and found that it was well correlated with some δ13C metrics. Surprisingly, a variety’s water potential regulation (specifically its minimum critical leaf water potential under water deficit) was strongly correlated to δ13C values under well-watered conditions, suggesting that base WUE may have a stronger impact on drought tolerance than WUE under water deficit. These results give strong insights on the innate WUE of a very large panel of varieties and suggest that studies of drought tolerance should include traits expressed under non-limiting conditions.

Green berries on Gewürztraminer (Vitis vinifera L.) in South Tyrol (Italy)

The grape variety Gewürztraminer is known to be affected by two physiological disorders namely berry shrivel and bunch stem necrosis. During the season 2014 we noticed a new symptomatology type of ripening disorder on the variety. The new symptom showed not all berries fallowing the normal maturation stages, but single berries remaining at a soft but green stage till harvest. The broad distribution of these so called “green berries” symptoms in different production sites of our region, caused huge damage due to the difficulty of eliminating single berries per bunch before harvesting. Therefore, the Research Centre Laimburg began to investigate the reasons and origins of this new symptom. This work shows the results of first attempts to find causes for the symptom as well as the resulting approach to mitigate symptoms. Applications of magnesium leaf fertilizer showed first promising results against this putative disorder. To study the causal effect of the green berries 30 symptomatic vineyards in 2014 have been selected for a monitoring during the season 2016. To evaluate the foliar nutrient treatment two vineyards have been selected for application of magnesium sulfate and magnesium chloride. Leaf and berry nutrient analysis, as well as the main quality parameters during ripening have been performed. As soon as “green berries” symptoms appeared, incidence and severity have been evaluated. Most of the symptomatic vineyards of the 2016 monitoring showed light to clear magnesium deficit symptoms on their foliage. Only during the seasons 2020 and 2021 “green berries” symptoms could be found in the leaf fertilizer treatment vineyards. Both seasons showed a significant effect of the magnesium treatments to reduce the incidence and severity of the symptom. It seems that the appearance of the “green berries” symptom on Gewürztraminer is correlated to a disturbed uptake of magnesium of the vines.

Effect of multi-level and multi-scale spectral data source on vineyard state assessment

Currently, the main goal of agriculture is to promote the resilience of agricultural systems in a sustainable way through the improvement of use efficiency of farm resources, increasing crop yield and quality under climate change conditions. This last is expected to drastically modify plant growth, with possible negative effects, especially in arid and semi-arid regions of Europe on the viticultural sector. In this context, the monitoring of spatial behavior of grapevine during the growing season represents an opportunity to improve the plant management, winegrowers’ incomes, and to preserve the environmental health, but it has additional costs for the farmer. Nowadays, UAS equipped with a VIS-NIR multispectral camera (blue, green, red, red-edge, and NIR) represents a good and relatively cheap solution to assess plant status spatial information (by means of a limited set of spectral vegetation indices), representing important support in precision agriculture management during the growing season. While differences between UAS-based multispectral imagery and point-based spectroscopy are well discussed in the literature, their impact on plant status estimation by vegetation indices is not completely investigated in depth. The aim of this study was to assess the performance level of UAS-based multispectral (5 bands across 450-800nm spectral region with a spatial resolution of 5cm) imagery, reconstructed high-resolution satellite (Sentinel-2A) multispectral imagery (13 bands across 400-2500 nm with spatial resolution of <2 m) through Convolutional Neural Network (CNN) approach, and point-based field spectroscopy (collecting 600 wavelengths across 400-1000 nm spectral region with a surface footprint of 1-2 cm) in a plant status estimation application, and then, using Bayesian regularization artificial neural network for leaf chlorophyll content (LCC) and plant water status (LWP) prediction. The test site is a Greco vineyard of southern Italy, where detailed and precise records on soil and atmosphere systems, in-vivo plant monitoring of eco-physiological parameters have been conducted.

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.