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…

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.

USING CHECK-ALL-THAT-APPLY (CATA) TO CATEGORIZE WINES: A DECISION-MAKING TOOL FOR WINE SELECTION

Bordeaux is the largest appellation vineyard in France. This contrasting vineyard with varied terroirs offers all styles of wine, resulting from the blending of several grape varieties. If these different profiles make the renown of Bordeaux wines, it can appear as a constraint when the aim is to study Bordeaux wines in their diversity. The selection of a representative sample can be performed by a sensory analysis carried out by trained panelists or by wine professionals, which can take several forms: consensus among experts, conventional descriptive analysis, typicality or quality evaluation. However, because of time, economic, and logistical constraints, these methods have limited applications. As an alternative to classical descriptive analysis, more intuitive methods that do not require training have been proposed recently to describe wines using an expert panel such as Napping, Free Choice or Flash Profiling, CATA or RATA.

WINE LEES AS A SOURCE OF NITROGEN FOR OENOCOCCUS OENI TO IMPROVE MALOLACTIC FERMENTATION PERFORMANCE

Malolactic fermentation (MLF) is a desired process in red and acidic white wines, after alcoholic fermentation (AF), carried out by the lactic acid bacterium (LAB) Oenococcus oeni. The advantages are an increase of pH, microbiological stabilization and organoleptic improvement of the final wine. However, the presence of stress factors such as ethanol, low pH, high total SO2, lack of nutrients and presence of inhibitors, could affect the successful completion of MLF [1]. Changes in amino acid composition and deficiencies in peptides after AF, showed that MLF can be delayed, signaling its importance for bacterial growth and L-malic acid degradation during MLF [2].

IMPACT OF MANNOPROTEIN N-GLYCOSYL PHOSPHORYLATION AND BRANCHING ON WINE POLYPHENOL INTERACTIONS WITH YEAST CELL WALLS

Yeast cell walls (CWs) may adsorb wine components with a significant impact on wine quality. When dealing with red wines, this adsorption is mainly related to physicochemical interactions between wine polyphenols and cell wall mannoproteins. However, mannoproteins are a heterogeneous family of complex peptidoglycans including long and highly branched N-linked oligosaccharides and short linear O-linked oligosaccharides, resulting in a huge structural diversity.

IMPACT OF CLIMATIC CONDITIONS ON THE SEASONING QUALITY OF OAK WOOD FOR OENOLOGICAL USE (QUERCUS PETRAEA)

For coopers, seasoning and toasting are considered crucial steps in barrel making during which the oak wood develops specific organoleptic properties. Seasoning, carried out in the open air, allows reducing the moisture content of the staves to between 14 and 18% (compared to 70 to 90% after splitting) while modulating the intrinsic composition of the oak wood. Toasting consists of applying different degrees of heat to a barrel for a specific period of time. As the temperature increases, oak wood produces a wide range of chemical compounds through thermal degradation of its intrinsic composition.