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…

MODELLING THE AGEING POTENTIAL OF SYRAH RED WINES BY ACCELERATED AGEING TESTS: INFLUENCE OF ANTIOXIDANT ASSAYS AND PHENOLIC COMPOSITION

Red wine ageing is an important step in the red wine evolution and impacts its chemical and sensory characteristics through many chemicals and physico-chemical reactions. The kinetics of these evolutions depend on the wine studied and influence the wine ageing potential. Generally, high quality red wines require a longer period of bottle ageing before consumption¹. The ageing potential is an impor-tant parameter for wine quality and is related to the capacity of a wine to undergo oxidation over time². Phenolic compounds which are ones of the main substrates for oxidation can then potentially modulate ageing potential³.

INVESTIGATION OF MALIC ACID METABOLIC PATHWAYS DURING ALCOHOLIC FERMENTATION USING GC-MS, LC-MS, AND NMR DERIVED 13C-LABELED DATA

Malic acid has a strong impact on wine pH and the contribution of fermenting yeasts to modulate its concentration has been intensively investigated in the past. Recent advances in yeast genetics have shed light on the unexpected property of some strains to produce large amounts of malic acid (“acidic strains”) while most of the wine starters consume it during the alcoholic fermentation. Being a key metabolite of the central carbohydrate metabolism, malic acid participates to TCA and glyoxylate cycles as well as neoglucogenesis. Although present at important concentrations in grape juice, the metabolic fate of malic acid has been poorly investigated.

CHARACTERIZATION OF ENOLOGICAL OAK TANNIN EXTRACTS BY MULTI-ANALYTICAL METHODS APPROACH

Oak tannin extracts are commonly used to improve wine properties. The main polyphenols found in oak wood extracts are ellagitannins¹ that release ellagic acid upon hydrolysis and comprise numerous structures². Moreover, oak tannin extracts contain other compounds giving a complex mixture. Consequently, the official OIV method based on gravimetric analysis of the tannin fraction adsorbed on polyvinylpolypyrrolidone is not sufficient to describe their composition and highlight their chemical diversity.

EFFECT OF WHOLE BUNCH VINIFICATION ON THE ABUNDANCE OF A SWEETENING COMPOUND

In classic red wine-making process, grapes are usually destemmed between harvest and the filling of the vat. However, some winemakers choose to let all or a part of the stems in contact with the juice during vatting, this is called whole bunch vinification. For instance, this practice is traditionally used in some French wine regions, notably in Burgundy, Beaujolais and the Rhone Valley. The choice to keep this part of the grape is likely to affect the sensory properties of wine, as its gustatory perception1,2.

PRODUCTION OF A FUNCTIONAL BEVERAGE FROM WINEMAKING BY-PRODUCTS: A NEW WAY OF VALORISATION

In the challenge of transforming waste into useful products that can be re-used in a circular economy perspective, winery by-products can be considered as a source of potentially bioactive molecules such as polyphenols. The wine industry generates each year 20 million tons of by-products. Kombucha fermentation is an ancestral process which allow to increase the biological properties of tea by the action of a microbial consortium formed by yeasts and bacteria called SCOBY. It belongs to the field of healthy food for which the interest of consumers is growing. The objective of this work was to propose a new functional beverage made from winemaking by-products fermented by a Kombucha SCOBY.