Integrating analytical resolutions in non-targeted wine metabolomics

Direct injection Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS), and ultra-high performance liquid chromatography coupled to mass spectrometry (UPLC/MS) were combined for the non-targeted analysis of wine metabolites. The unrivalled resolution on mass measurement allowed by the former and the separation ability of isomeric and isobaric substances by the latter, clearly increases the scope of detectable unknown metabolites in wines. Such methodology is illustrated through the comparison of chemical spaces of a young and an older Pinot noir wine. RP and HILIC chromatography could reveal up to five isomers for a given mass, throughout the explored mass range. CHO, CHOS …

Polyphenols in kombucha: Metabolomic analysis of biotransformations during fermentation

Kombucha is a non-alcoholic beverage made of sugared tea that is transformed by a symbiotic consortium of yeasts and bacteria. This beverage is increasingly produced at industrial scale, but its quality standards remain to be defined. Metabolomics analysis was carried out using FT-ICR-MS (Fourier Transform-Ion Cyclotron Resonance-Mass Spectrometry) to understand the chemical transformations induced by the production phases and the type of tea on the non-volatile compounds of kombucha.

Natural oxygenation of Champagne wine during ageing on lees: A metabolomics picture of hormesis

International audience; The oxygenation of Champagne wine after 4 and 6 years of aging on lees in bottle was investigated by FTICR-MS and UPLC-Q-TOF-MS. Three levels of permeability were considered for the stoppers, ranging from 0.2 to 1.8 mg/L/year of oxygen transfer rate. Our results confirmed a good repeatability of ultrahigh resolution FTICR-MS, both in terms of m/z and coefficient of variation of peak intensities among biological replicates. Vintages appeared to be the most discriminated features, and metabolite annotations suggested that the oldest wines (2006) were characterized by a higher sensitivity towards oxygenation. Within each vintage, the oxygenation mechanisms appeared to b…

Yeast interaction on Chardonnay wine composition: Impact of strain and inoculation time.

Abstract It is of great importance to understand the molecular characteristics and substantial chemical transformations due to yeast-yeast interaction. Non-targeted metabolomics was used to unravel must in fermentation composition, inoculated with non-Saccharomyces (NS) yeasts and Saccharomyces cerevisiae (S) for sequential fermentation. ultrahigh-resolution mass spectrometry was able to distinguish thousands of metabolites and provides deep insights into grape must composition allowing better understanding of the yeast-yeast interactome. The dominance of S, characterized by a metabolic richness not found with NS, is dependent on inoculation time and on the yeast species present. Co-inocula…

A grape and wine chemodiversity comparison of different appellations in Burgundy: vintage vs terroir effects.

Abstract This study aimed at assessing the ability of high resolution Fourier Transform Ion Cyclotron Resonance – Mass Spectrometry (FTICR–MS) to differentiate grapes and corresponding wines from distinct vineyards managed by a same producer, according to complex chemical fingerprints. Grape extracts (at harvest) and corresponding wines from four different vineyards, sampled immediately after the alcoholic fermentation over three successive vintages, were analysed by FTICR–MS. Thousands of metabolites that are specific to a given vintage, or a given class (wine, skin or must) could be revealed, thus emphasising a strong vintage effect. The same wines were reanalyzed after a few years in bot…

Chemical messages in 170-year-old champagne bottles from the Baltic Sea: Revealing tastes from the past

International audience; Archaeochemistry as the application of the most recent analytical techniques to ancient samples now provides an unprecedented understanding of human culture throughout history. In this paper, we report on a multiplatform analytical investigation of 170-y-old champagne bottles found in a shipwreck at the bottom of the Baltic Sea, which provides insight into winemaking practices used at the time. Organic spectroscopy-based nontargeted metabolomics and metallomics give access to the detailed composition of these wines, revealing, for instance, unexpected chemical characteristics in terms of small ion, sugar, and acid contents as well as markers of barrel aging and Maill…

Vitamins in wine: Which, what for, and how much?

Vitamins are essential compounds to yeasts, and notably in winemaking contexts. Vitamins are involved in numerous yeast metabolic pathways, including those of amino acids, fatty acids, and alcohols, which suggests their notable implication in fermentation courses, as well as in the development of aromatic compounds in wines. Although they are major components in the course of those microbial processes, their significance and impact have not been extensively studied in the context of winemaking and wine products, as most of the studies focusing on the subject in the past decades have relied on relatively insensitive and imprecise analytical methods. Therefore, this review provides an extensi…

How subtle is the "terroir" effect? Chemistry-related signatures of two "climats de Bourgogne".

The chemical composition of grape berries is influenced by various environmental conditions often considered to be representative of a "terroir". If grapes from a given terroir are assumed to reflect this origin in their chemical compositions, the corresponding wine should also reflect it. The aim of this work was therefore to reveal the "terroir" expression within the chemodiversity of grapes and related wines, using ultrahigh-resolution mass spectrometry. Grapes and corresponding wines, from two distinct - though very proximate - terroirs of Burgundy were analyzed over three vintages (2010, 2011 and 2012). Ultrahigh-resolution mass spectrometry and ultra-high performan…

Influence of regionality and maturation time on the chemical fingerprint of whisky.

International audience; Understanding the chemical composition of whisky and the impact of each step in the manufacturing process provides a basis for responding to the challenges of producing high quality spirits. In this study, the objective was to discriminate whiskies according to their geographical origin and authenticate the maturation time in cask based on the non-volatile profiles. The combination of FT-ICR-MS and chemometrics allowed the distinction of whiskies from four geographical origins in Scotland (Highlands, Lowlands, Speyside and Islay). Statistical modeling was also used to discriminate whiskies according to the maturation time in cask and reveal chemical markers associate…

Chemical messages from an ancient buried bottle: Metabolomics for wine archeochemistry.

Restoration works in the old Clunisian Saint-Vivant monastery in Burgundy revealed an unidentified wine bottle (SV1) dating between 1772 and 1860. Chemical evidence for SV1 origin and nature are presented here using non-targeted Fourier Transform Ion Cyclotron Resonance Mass Spectrometry and Nuclear Magnetic Resonance analyses. The SV1 chemical diversity was compared to red wines (Pinot Noir) from the Romanée Saint Vivant appellation and from six different vintages spanning from 1915 to 2009. The close metabolomic signature between SV1 and Romanée Saint Vivant wines spoke in favor of a filiation between these wines, in particular considering the Pinot noir grape variety. A further statistic…

Combined Nontargeted Analytical Methodologies for the Characterization of the Chemical Evolution of Bottled Wines

Fluorescence fingerprinting of bottled white wines can reveal memories related to sulfur dioxide treatments of the must.

For the first time, Excitation Emission Matrix (EEM) fluorescence spectroscopy was combined with parallel factor statistical analysis (PARAFAC) and applied to a set of 320 dry white wines of the Chardonnay grape variety. A four component PARAFAC model (C1, C2, C3 and C4) best explained the variability of fluorescence signatures of white wines. Subtle changes were observed in EEMs of white wines from two different vintages (2006 and 2007), where different concentrations of sulfur dioxide (0, 4, and 8 g·hL(-1)) were added to the grape must at pressing. PARAFAC results clearly indicated that sulfur dioxide added to the must subsequently influenced white wine chemistry into three distinct sulfu…

Cultivar- and Wood Area-Dependent Metabolomic Fingerprints of Grapevine Infected by Botryosphaeria Dieback

International audience; Botryosphaeria dieback is one of the most significant grapevine trunk diseases that affects the sustainability of the vineyards and provokes economic losses. The causal agents, Botryosphaeriaceae species, live in and colonize the wood of the perennial organs causing wood necrosis. Diseased vines show foliar symptoms, chlorosis, or apoplexy, associated to a characteristic brown stripe under the bark. According to the susceptibility of the cultivars, specific proteins such as PR-proteins and other defense-related proteins are accumulated in the brown stripe compared with the healthy woody tissues. In this study, we enhanced the characterization of the brown stripe and …

Un message du passé viticole de la Bourgogne : la bouteille découverte dans l’abbaye Saint-Vivant de Vergy (Côte-d’Or)

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Structural studies of adsorbed protein (betalactoglobulin) on natural clay (montmorillonite)

International audience; In this work, the adsorption of a small globular protein (betalactoglobulin, BLG), on a natural montmorillonite clay (Mt) was investigated in acidic buffer (pH = 3). The combination of different characterization techniques such as zetametry, X-ray diffraction, transmission electronic microscopy, fluorescence and solid state nuclear magnetic resonance spectroscopies shed light on the interaction mechanism between the clay mineral and the proteins. For low BLG concentration, a slight increase of the interlayer spacing of the clay mineral was noticed as well as structural changes of the protein. In contrast, as the concentration of BLG increased, the adsorption led to a…

Wine metabolomic analysis : "chemical messages in a bottle"

The main objective of this work was to develop non-targeted metabolomics analyses of bottled wines in order to decipher chemical informations from the time-related evolution of their composition. This original research was based on the hypothesis that, when analyzed, bottled wines would still hold chemical memories of envionmental parameters (vineyard management, oenological practices, climate, terroir…) at the moment of their elaboration, even after several years of ageing. A second hypothesis was that in order to anticipate the future evolution of the wine quality in terms of chemical composition, it is necessary to know what it was in the past. To that purpose, and for the first time in …

Foodomics assessed by Fourier transform mass spectrometry

Abstract With its ultrahigh resolution power and excellent mass accuracy, Fourier transform ion cyclotron resonance mass spectrometry is the perfct tool to analyze the “foodome” as the set of all polar small molecular compounds present in an investigated food sample. We present here selected applications of this technique in unraveling the metabolome in complex foods (thermally affected, fermentation products, distillates) such exemplified with Maillard reaction products or with wines and spirits. Technical considerations for high resolution mass analyzers are provided from a practical point of view. Moreover, aspects of food safety and nutritional quality are covered by presenting applicat…

Sulfites and the Wine Metabolome

International audience; In a context of societal concern about food preservation, the reduction of sulfite input plays a major role in the wine industry. To improve the understanding of the chemistry involved in the SO2 protection, a series of bottle aged Chardonnay wines made from the same must, but with different concentrations of SO2 added at pressing were analyzed by ultrahigh resolution mass spectrometry (FT-ICR-MS) and excitation emission matrix fluorescence (EEMF).Metabolic fingerprints from FT-ICR-MS data could discriminate wines according to the added concentration to the must but they also revealed chemistry-related differences according to the type of stopper, providing a wine me…

"Omics-" for a mapping of grapevine response to elicitors and identification of induced resistance markers

SPEIPMINRAUBCNRS; "Omics-" for a mapping of grapevine response to elicitors and identification of induced resistance markers . 12. European Fondation for Plant Pathology (EFPP) & 10. French Society for Plant Pathology Conference ‘Deepen Knwoledge in Plant Pathology for Innovative Agro-Ecology’

Influence of cell-cell contact between L. thermotolerans and S. cerevisiae on yeast interactions and the exo-metabolome

International audience; Sequential fermentation of grape must inoculated with L. thermotolerans and then S. cerevisiae 24 h later (typical wine-making practice) was conducted with or without cell-cell contact between the two yeast species. We monitored cell viability of the two species throughout fermentation by flow cytometry. The cell viability of S. cerevisiae decreased under both conditions, but the decrease was greater if there was cell-cell contact. An investigation of the nature of the interactions showed competition between the two species for nitrogen compounds, oxygen, and must sterols. Volatile-compound analysis showed differences between sequential and pure fermentation and that…