Targeted and untargeted 1H-NMR analysis for sparkling wine’s authenticity

Purpose of this research is to quantitatively assess the mineral component of vineyard soils, with particular attention to the mineralogical analysis of clays, which represent an element of high importance in the vineyard culture as well as in general agriculture. An X-ray diffraction (XRD) / thermogravimetric (TG) multi-technique analytical approach was developed, tested on soil samples taken from vineyards around the world. This codified analytical procedure was necessary to obtain precise qualitative and quantitative mineralogical data, globally comparable to distinguish the geopedological identity of the vineyards. Soil samples from vineyards of various locations were analysed, in very different geological conditions. The bulk-rock quantitative phase analysis (QPA) was obtained by the Rietveld method while the detailed composition of the clay-sized fraction was determined by modelling of the oriented X-ray diffraction patterns. The research provided a precise classification of the mineral component of soils, distinguishing the mineral phases of the clays and the so-called mixed-layer clay minerals. We found that the content in mixed layers can be directly correlated with the water retention and the cation exchange capacity ​​of the soil, while the presence of other clayey minerals and phyllosilicates in this research did not affect this CEC parameter, which codes the fertility level of the soils. The study demonstrates that terroir, in particular soils formed in complex or very different geological conditions, can only be effectively interpreted by properly analysing its mineral phases, in particular the mixed-layer clay component. These are characteristic abiotic ecological indicators, which may have specific eco-physiological influences on the plant.

Protected Designation of Origin “Jumilla” (PDO Jumilla) is located in the Spanish provinces of Albacete and Murcia, in the South-eastern part of the Iberian Peninsula, where most of the models predict a severe impact of climate change in next decades. PDO Jumilla covers an area of 247,054 hectares, of which more than 22,000 hectares

Climate change and rising atmospheric carbon dioxide concentration is a concern for agriculture, including viticulture. Studies on elevated carbon dioxide have already been on grapevines, mainly taking place in greenhouses using potted plants or using field grown vines under higher CO2 enrichment, i.e. >650 ppm. The VineyardFACE, located at Hochschule Geisenheim University, is an open field Free Air CO2 Enrichment (FACE) experimental set-up designed to study the effects of elevated carbon dioxide using field grown vines (Vitis vinifera L. cvs. Riesling and Cabernet Sauvignon). As the carbon dioxide fumigation started in 2014, the long term effects of elevated carbon dioxide treatment can be investigated on berry ripening parameters and fruit metabolic composition.
The present study aims to investigate the effect on fruit composition under a moderate increase (+20%; eCO2) of carbon dioxide concentration, as predicted for 2050 on both Riesling and Cabernet Sauvignon. Berry composition was determined for primary (sugars, organic acids, amino acids) and secondary metabolites (anthocyanins). Special focus was given on monitoring of berry diameter and ripening rates throughout three growing seasons. Compared to previous results of the early adaptative phase of the vines [1], our results show little effect of eCO2 treatment on primary metabolites composition in berries. However, total anthocyanins concentration in berry skin was lower for eCO2 treatment in 2020, although the ratio between anthocyanins derivatives did not differ.
[1] Wohlfahrt Y., Tittmann S., Schmidt D., Rauhut D., Honermeier B., Stoll M. (2020) The effect of elevated CO2 on berry development and bunch structure of Vitis vinifera L. cvs. Riesling and Cabernet Sauvignon. Applied Science Basel 10: 2486

The first demonstration of the interest of carbon isotope composition of sugars in grapevine, as an integrated indicator of vineyard water status, dates back to 2000 (Gaudillère et al., 1999; Van Leeuwen et al., 2001). Thanks to the isotopic discrimination of Carbon that takes place during plant photosynthesis, under hydric stress conditions, it is possible to accurately estimate the photosynthetic activity. Ever since, δ13C has been widely applied with success to zonation, terroir studies and vine physiology research, but is still not widely used by viticulturists. This is quite astonishing by considering the impact of global warming on viticulture and the need to improve water management, that would justify a widespread use of δ13C.
The lack of private laboratories proposing the analysis, the cost of the technology, as well as the long analytical delays, have been detrimental to its development. Some laboratories tried to overcome the analytical difficulties of isotopic analysis by using fourier transformed infrared spectroscopy, as a fast and cheap alternative to the official OIV method (IRMS). These claimed FTIR models have never been published or peer reviewed and cannot be considered robust. In this work, thanks to the recent acquisition of IRMS technology, new modern and robust applications of δ13C for viticulture are proposed. This includes the use of the analysis to make parcel separations at harvesting, the possibility to increase the precision of hydric stress cartography and the potential cost reduction when compared with Scholander pressure bomb analysis.

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.