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…

MAPPING OF GAS-PHASE CO₂ IN THE HEADSPACE OF CHAMPAGNE GLASSES BY USING AN INFRARED LASER SENSOR UNDER STATIC TASTING CONDITIONS

From the chemical angle, Champagne wines are complex hydro-alcoholic mixtures supersaturated with dissolved carbon dioxide (CO₂). During the pouring process and throughout the several minutes of tasting, the headspace of a champagne glass is progressively invaded by many chemical species, including gas-phase CO₂ in large majority. CO₂ bubbles nucleated in the glass and collapsing at the champagne surface act indeed as a continuous paternoster lift for aromas throughout champagne or sparkling wine tasting [1]. Nevertheless, inhaling a gas space with a concentration of gaseous CO₂ close to 30% and higher triggers a very unpleasant tingling sensation, the so-called “carbonic bite”, which might completely perturb the perception of the wine’s bouquet.

METHYL SALICYLATE: A TRENDY COMPOUND MARKER OF ZELEN, A UNIQUE SLOVENIAN VARIETY

The wine market interest for autochthonous varieties, particularly from less known wine regions, has significantly raised in the past few years. In that context, Slovenia, a small country from central Europe with a long winemaking tradition, is getting more and more attention, particularly through its range of unique regional varieties. Among them, Zelen, meaning “green” in Slovene, can only be found in the Vipava valley region, located on the western side of the country, near the border with Italy. When they are young, Zelen wines display very singular aromas reminiscent of rosemary, sage and white fruit. Despite its uniqueness, Zelen wine aromatic typicality is poorly documented in the literature.

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].

EVOLUTION OF CHEMICAL AND SENSORIAL PROFILE OF WINES ELABORATED WITH THEIR OWN TOASTED VINE-SHOOTS AND MICRO-OXYGENATION

The positive contribution of toasted vine-shoots (SEGs, Shoot from vines – Enological – Granule) used in winemaking to the chemical and sensory profile of wines has been widely proven. However, the combination of this new enological tool with other winemaking technologies, such as micro-oxygenation (MOX), has not been studied so far. It is known that micro-oxygenation is used in wineries to stabilizes color, improves structure or combining with oak alternatives products to achieve a more effective aroma integration of wines. For that, its implementation in combination with SEGs could result in differentiated wines.

BIOSORPTION OF UNDESIRABLE COMPONENTS FROM WINE BY YEAST-DERIVED PRODUCTS

4-Ethylphenol (EP) in wine is associated with organoleptic defects such as barn and horse sweat odors. The origin of EP is the bioconversion reaction of p-coumaric acid (CA), naturally present in grapes and grape musts by contaminating yeasts of the genus Brettanomyces bruxellensis.
Yeast cell walls (YCW) have shown adsorption capacities for different compounds. They could be applied to wines in order to adsorb either CA and/or EP and thus reduce the organoleptic defects caused by the contaminating yeasts.