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…

INTENSE PULSED LIGHT FOR VINEYARD WASTEWATER: A PROMISING NEW PROCESS OF DEGRADATION FOR PESTICIDES

The use of pesticides for vine growing is responsible for generating an important volume of wastewater. In 2009, 13 processes were authorized for wastewater treatment but they are expensive and the toxicological impact of the secondary metabolites that are formed is not clearly established. Recently photodecomposition processes have been studied and proved an effectiveness to degrade pesticides and to modify their structures (Maheswari et al., 2010, Lassale et al., 2014). In this field, Pulsed Light (PL) seems to be an interesting and efficient process (Baranda et al., 2017). Therefore, the aim of this work was to investigate the PL technology as a new process for the degradation of pesticides.

EXPLORING THE ROLE OF TRANSITION METAL IONS IN THE EVOLUTION OF ESTERS COMPOSITION OF YOUNG WHITE WINE DURING AGEING

Young white wines are typically released to the market a few months after harvest, to be consumed within a year, when their fresh fruity aromas are still dominant and appealing to modern consumers. Esters, particularly higher alcohol acetates (HAAs) and ethyl esters of fatty acids (EEFAs), play a central role in the fruity expression of young white wines [1]. However, these esters are known to undergo significant hydrolysis during the first months of aging [1, 2].

POTENTIAL DEACIDIFYING ROLE OF A COMMERCIAL CHITOSAN: IMPACT ON PH, TITRATABLE ACIDITY, AND ORGANIC ACIDS IN MODEL SOLUTIONS AND WHITE WINE

Chitin is the main structural component of a large number of organisms (i.e., mollusks, insects, crustaceans, fungi, algae), and marine invertebrates including crabs and shrimps. The main derivative of chitin is chitosan (CH), produced by N-deacetylation of chitin in alkaline solutions. Over the past decade, the OIV/OENO 338A/ 2009 resolution approved the addition of allergen-free fungoid CH to must and wine as an adjuvant for microbiological control, prevention of haziness, metals chelation and ochratoxins removal (European Commission. 2011). Despite several studies on application of CH in winemaking, there are still very limited and controversial data on its interaction with acidic components in wine (Colan-gelo et al., 2018; Castro Marin et al., 2021).

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].

OPTIMIZATION OF EXTRACTION AND DEVELOPMENT OF AN LC-HRMS METHOD TO QUANTIFY GLUTATHIONE IN WHITE WINE LEES AND YEAST DERIVATIVES

Glutathione is a natural tripeptide composed of l-glutamate, l-cysteine and glycine, found in various foods and beverages. In particular, glutathione can be found in its reduced (GSH) or oxidized form (GSSG) in must, wine or yeasts¹. Numerous studies have highlighted the importance of GSH in wine quality and aging potential². During winemaking, especially during aging on lees, GSH helps prevent the harmful effects of oxidation on the aroma of the wine³. Nevertheless, the amounts of GSH/GSSG present in wine lees are often unknown and the choice of operating conditions (quantity of lees and aging time) remains empirical.