Facing climate change in wine industry comprises the implementation of strategies, such as to reduce alcohol in wines, promoted by abnormal increment of sugar levels in wine grapes. The present work discusses the first industrial-scale use of specific yeast strains able to produce wine with reduced alcoholic concentration. Reduction of alcohol content and quantification of key metabolites associated to oenological practice and/or quality were simultaneously measured in a “one-shot” way with proton Nuclear Magnetic Resonance Spectroscopy. Novel relevant metabolites were revealed with the use of a two-dimensional 1H-13C HSQC multipresat correlation spectroscopy, whereas a detailed methodological NMR description is stressed, towards revealing novel resonances within the NMR signature. The use of multitask analytical methods to simultaneously describe alcohol reduction and NMR targeting, completes the portfolio of NMR solutions recently proposed to the World Organisation of Vine and Wine for as well quantify aging and varieties.

Since 1953, The World Organization of Vine and Wine (OIV) Member States have reduced the lead maximum limits (ML) in wines, down to 0.05 mg/L (2018). Evidently, this ML value is too restrictive for wine industry as it excludes from international market a significant portion of wine production. Currently, the Codex Committee on Contaminants in Foods and OIV had recognized the value of gathering robust and novel data to better assess the best lowest ML for wine industry. Currently, there is not a direct statement within international reference documents, of which chemical form of lead must be controlled and/ or reduced. This work presents for the first time a method combining Energy Dispersive X-Ray analysis (EDAX) and Nuclear Magnetic Resonance (NMR) spectroscopies in order to determine presence and concentrations of major and trace elements of lead and other element moieties in wine that can allow to better redefine lead's ML. By identification of K, L, M, radiation shells with additional αβi labelling of lead's major and minor components with semi-quantitative XRF, combined with chemical-shift analysis of inorganic Pb4+, Pb2+ and/or organo-lead within wine samples, we propose a full discrimination framework to disentangle and quantify different chemical forms of lead.

Present work discusses strengths and limitations of two Nuclear Magnetic Resonance outliers obtained with a water-to-ethanol solvent multi pre saturation acquisition method, recently included in the Compendium of International Methods of Analysis of Wines and Musts, published as OIV-MA-AS316-01, and their accuracy for metabolomics analysis. Furthermore, it is also presented an alternative to produce more discriminant and sensitive NMR data matrices for metabolomics studies, comprising the use of a novel NMR acquisition strategy in wines, the double pulsed-field gradient echo (DPFGE) NMR scheme, with a refocusing band-selective uniform-response pure-phase selective pulse, for a selective excitation of the 5-10 ppm chemical shift range of wine samples, that reveals novel broad aromatic 1H resonances, directly associated to complex polyphenols. Both aromatics and full binned OIV-MA-AS316-01,as well as the selective 5-10 ppm DPFGE NMR outliers were statistically analyzed with diverse non-supervised Principal Component Analysis (PCA) and supervised Partial Least Squares -Discriminant Analysis (PLS-DA), sparse (sPLS-DA) least squares- discriminant analysis, and orthogonal projections to latent structures discriminant analysis (OPLS-DA). Supervised multivariate statistical analysis of DPFGE and aromatics’ binned OIV-MA-AS316-01NMR data have shown their robustness to broadly discriminate geographical origins and narrowly differentiate between different fermentation schemes of wines from identical variety and region.