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…

WINE RACKING IN THE WINERY AND THE USE OF INERT GASES: CONTROL AND OPTIMIZATION OF THE PROCESS

Atmospheric oxygen (O₂) generates oxidation in wines that affect their physicochemical and sensory evolution. The O₂ uptake in the different winemaking processes is generally considered to be negative for the sensory characteristics of white and rosé wines. Wine racking is a critical point of O₂ uptake, as the large surface area of the wine exposed during this operation and the inability to maintain an effective inert gas blanket over it. The aim was to study the uptake of O₂ during the racking of a model wine as a reference and to compare with purging the destination tank with different inert gases.

EFFECTS OF LEAF REMOVAL AT DIFFERENT BUNCHES PHENOLOGICAL STAGES ON FREE AND GLYCOCONJUGATE AROMAS OF SKINS AND PULPS OF TWO ITALIAN RED GRAPES

Canopy-management practices are applied in viticulture to improve berries composition and quality, having a great impact on primary and secondary grape metabolism. Among these techniques, cluster zone leaf removal (defoliation) is widely used to manage air circulation, temperature and light radiation of grape bunches and close environment. Since volatiles are quantitatively and qualitatively influenced by the degree of fruit ripeness, the level of solar exposure, and the thermal environment in which grapes ripen, leaf removal has been shown to affect volatile composition of grape berries [1].

ADDITION OF OAK WOOD ALTERNATIVE PRODUCTS: QUALITATIVE AND SENSORIAL EFFECTS FOR A WHITE WINE OF ALIGOTE

Wines matured in contact with wood are extremely popular with consumers all over the world. Oak wood allows the organoleptic characteristics of wine to be modified. Wines are enriched with volatile and non-volatile compounds extracted from the wood. The aromas extracted from oak wood contribute to the construction of the wine’s aromatic profile and the main polyphenols extracted can modify taste perceptions such as astringency and bitterness. All the compounds extracted from the wood thus contribute to the balance and quality of the wines.

NEW PLANT BIOPOLYMERS FOR THE COLLOIDAL STABILITY OF THE COLORING MATTER OF RED WINES

The color as well as the “clarity” of red wines are ones of the qualities required by the consumers. Red wines must have colloidal stability from its bottling to its consumption. The supplementation of red wines with additives, and especially Acacia senegal gum, contributes to its organoleptic properties such as the colloidal stabilization of the coloring matter. In a global perspective of limitation of additives in the field of enology, one of the objectives is notably (i) to reduce the use of additives in wines, by their number and/or their quantity, and (ii) to favor the use of natural additives while preserving the organoleptic and sensory qualities of wines.

THE EFFECT OF COPPER ON THE PRODUCTION OF VARIETAL THIOLS DURING THE ALCOHOLIC FERMENTATION OF COLOMBARD AND GROS MANSENG GRAPE JUICES

Nowadays, the rapid growth of vineyards with organic practices and the use of copper as the only fun-gicide against downy mildew raises again the question of the effect of copper on varietal thiols in wine, especially 3-sulfanylhexan-1-ol (3SH) and its acetate (3SHA). A few decades ago, several works indicated that the use of copper in the vineyard had a negative effect on the content of varietal thiols in Sauvignon blanc wines [1, 2]. However, these studies only considered the concentration of the reduced form (RSH) of varietal thiols, without quantifying the oxidised ones. For this purpose, we proposed to monitor both reduced and oxidised forms of varietal thiols in wine under copper stress during alcoholic fermentation to have a more complete picture of the biological and chemical mechanisms.