terclim by ICS banner
IVES 9 IVES Conference Series 9 USE OF 13C CP/MAS NMR AND EPR SPECTROSCOPIC TECHNIQUES TO CHARACTERIZE MACROMOLECULAR CHANGES IN OAK WOOD(QUERCUS PETRAEA) DURING TOASTING

USE OF 13C CP/MAS NMR AND EPR SPECTROSCOPIC TECHNIQUES TO CHARACTERIZE MACROMOLECULAR CHANGES IN OAK WOOD(QUERCUS PETRAEA) DURING TOASTING

Abstract

For coopers, toasting process is considered a crucial step in barrel production during which oak wood (Q. petraea) develops several aromatic nuances released to the wine during its maturation. Toasting consists of applying different degrees of heat to a barrel for a specific period. As the temperature increases, thermal degradation of oak wood structure produces a huge range of chemical compounds. Many studies have identified the main key aroma volatile compounds (whisky-lactone, furfural, eugenol, guaiacol, vanillin). However, detailed information on how the chemical structure of oak wood degrades with increasing toasting level is still lacking.

In this study, we characterised the structural changes of the main components (cellulose, hemicellulose and lignin) of oak wood staves subjected to heat treatments (non-toasted to 240 °C) by cross-polarisation/magic angle spinning nuclear magnetic resonance (CP/MAS NMR, 800 MHz) and electron para-magnetic resonance (EPR, X-band) spectroscopy techniques applied to solids. Furthermore, the results will be compared to those obtained by quantitative GC-MS (EI) analysis of oak wood volatile compounds generated by the same heat treatments. The 13C CP/MAS NMR data highlighted concomitant phenomena of demethoxylation and depolymerisation of syringyl units leading to the formation of guaiacyl units and the release of monomer units. EPR results revealed the same phenomena and led us to hypothesize that the nature of the radical formed evolved during toasting from syringyl to guaiacyl form. Our results are consistent with data on others wood species and confirm that 200 °C is a threshold temperature above which degradation of the macromolecular structure leads to the formation of radicals and volatile compounds. Overall, the study offers interesting perspectives for the application of spectroscopic techniques, particularly EPR spectroscopy, to monitor radical formation during barrel aging and, consequently, to assess the oxidative stability of wine.

DOI:

Publication date: February 9, 2024

Issue: OENO Macrowine 2023

Type: Poster

Authors

Marie Courregelongue 1,2,3, Mathieu Duttine ⁴, Axelle Grélard ⁵, Alexandre Pons 1,2,3

1. Univ. Bordeaux, Bordeaux INP, INRAE, OENO, UMR 1366, ISVV, F-33140 Villenave d’Ornon, France
2. Bordeaux Sciences Agro, F-33170 Gradignan, France
3. Seguin Moreau Cooperage, ZI Merpins, F-16103 Cognac, France
4. Univ. Bordeaux, CNRS, Bordeaux INP, ICMCB, UMR 5026, F-33600 Pessac, France
5. Univ. Bordeaux, CNRS, Bordeaux INP, CBMN, UMR 5248, IECB, F-33600 Pessac, France

Contact the author*

Keywords

oak wood, thermal degradation, macromolecular components, aroma compounds

Tags

IVES Conference Series | oeno macrowine 2023 | oeno-macrowine

Citation

Related articles…

MONITOR SOME KEY PARAMETERS THROUGH THE IMPLEMENTATION OFCONTINUOUS CONTROL SYSTEMS OF THE MUST-WINE DURING MACERATION-FERMENTATION IN RED WINEMAKING TO MANAGE OPERATIONS IN “AUTOMATION”

This study is aimed to develop a complete tool for the winemaker with, complete and targeted “winemaking recipes” that can be adapted to criteria set by the winemaker, such as: grape variety, grape health status, degree of ripening, desired wine, redox status throughout the alcoholic fermentation. To get such aim, specific sets of experiments using red grape juices from different varieties (Nebbiolo, Barbera, Pinot noir, etc.) collected at different technological and phenolic maturity points, will be held with “automatized 4.0 tanks” equipped with sensors for measuring: redox potential, dissolved oxygen, relative density, temperature, and color in order to collect a sufficient amount of data preparatory to the creation of operating models in the most widely winemaking situations in which the automatized 4.0 tanks “will be able to independently respond” with the right corrective actions (opening/closing aeration valve, execution/block pumping overs , etc.) if the key parameters exceed the limits of the recommended ranges set in the selected recipe.

WINE WITHOUT ADDED SO₂: OXYGEN IMPACT AND EVOLUTION ON THE POLYPHENOLIC COMPOSITION DURING RED WINE AGING

SO₂ play a major role in the stability and wine during storage. Nowadays, the reduction of chemical input during red winemaking and especially the removing SO₂ is a growing expectation from the consumers. Winemaking without SO₂ is a big challenge for the winemakers since the lack of SO₂ affects directly the wine chemical evolution such as the phenolic compounds as well as its microbiological stability.

VOLATILE COMPOSITION OF WINES USING A GC/TOFMS: HS-SPME VS MICRO LLE AS SAMPLE PREPARATION METHODOLOGY

Wine aroma analysis can be done by sensorial or instrumental analysis, the latter involving several me-thodologies based on olfactometric detection, electronic noses or gas chromatography. Gas Chromatography has been widely used for the study of the volatile composition of wines and depending on the detection system coupled to the chromatographic system, quantification and identification of individual compounds can be achieved.

INFLUENCE OF GRAPE RIPENESS ON MACROMOLECULES EXTRACTABILITY FROM GRAPE SKIN TISSUES AND GRAPE SEEDS DURING WINEMAKING

A consequence of climate change is the modification of grape harvest quality and physico-chemical parameters of the obtained wine: increase in alcoholic degree, decrease in pH, and modification of the extractability of macromolecules, which leads to problems of microbiological, tartaric, colour and colloidal stability. In order to respond to these problems, the winemaking processes must be anticipated and adapted with a better knowledge of macromolecule extractability in grapes and their evolution, according to the grape variety, vintage and winemaking process. The purpose of this study was to understand 1) how the harvest date can influence the extractability of macromolecules, polysaccharides and phenolic compounds, which are responsible for wine stability 2) how to adapt the winemaking process to the harvest date in order to optimise wine quality.

YEAST-PRODUCED VOLATILES IN GRAPE BASED SYSTEM MODEL ACTING AS ANTIFUNGAL BIOAGENTS AGAINST PHYTOPATHOGEN BOTRYTIS CINEREA

Botrytis cinerea Pers., the causal agent of grey mould disease, is responsible for substantial economic losses, as it causes reduction of grape and wine quality and quantity. Exploitation of antagonistic yeasts is a promising strategy for controlling grey mould incidence and limiting the usage of synthetic fungicides. In our previous studies, 119 different indigenous yeasts were screened for putative multidimensional modes of action against filamentous fungus B. cinerea [1]. The most promissing biocontrol yeast was Pichia guilliermondii ZIM624, which exhibited several anatagonistic traits (production of cell wall degrading enzymes, chitinase and β-1,3-glucanase; demonstration of in vitro inhibitory effect on B. cinerea mycelia radial growth; production of antifungal volatiles, assimilation of a broad diversity of carbon sources, contributing to its competitivnes in inhabiting grapes in nature).