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…

REMEDIATION OF SMOKE TAINTED WINE USING MOLECULARLY IMPRINTED POLYMERS

In recent years, vineyards in Australia, the US, Canada, Chile, South Africa and Europe have been exposed to smoke from wildfires. Wines made from smoke-affected grapes often exhibit unpleasant smoky, ashy characters, attributed to the presence of smoke-derived volatile compounds, including volatile phenols (which occur in free and glycosylated forms). Various strategies for remediation of smoke tainted wine have been evaluated. The most effective strategies involve the removal of smoke taint compounds via the addition of adsorbent materials such as activated carbon, which can either be added directly or used in combination with nanofiltration. However, these treatments often simultaneously remove wine constituents responsible for desirable aroma, flavour and colour attributes.

DEVELOPMENT OF BIOPROSPECTING TOOLS FOR OENOLOGICAL APPLICATIONS

Wine production is a complex biochemical process that involves a heterogeneous microbiota consisting of different microorganisms such as yeasts, bacteria, and filamentous fungi. Among these microorganisms, yeasts play a predominant role in the chemistry of wine, as they actively participate in alcoholic fermentation, a biochemical process that transforms the sugars in grapes into ethanol and carbon dioxide while producing additional by-products. The quality of the final product is greatly influenced by the microbiota present in the grape berry, and the demand for indigenous yeast starters adapted to specific grape must and reflecting the biodiversity of a particular region is increasing. This supports the concept that indigenous yeast strains can be associated with a “terroir”.

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.

IDENTIFYING POTENTIAL CHEMICAL MARKERS RESPONSIBLE FOR THE PERMISSIVENESS OF BORDEAUX RED WINES AGAINST BRETTANOMYCES BRUXELLENSIS USING UNTARGETED METABOLOMICS

All along the red winemaking process, many microorganisms develop in wine, some being beneficial and essential, others being feared spoilers. One of the most feared microbial enemy of wine all around the world is Brettanomyces bruxellensis. Indeed, in red wines, this yeast produces volatile phenols, molecules associated with a flavor described as “horse sweat”, “burnt plastic” or “leather”. To produce significant and detectable concentrations of these undesired molecules, the yeasts should first grow and become numerous enough. Even if the genetic group of the strain present and the cellar temperature may modulate the yeast growth rate¹ and thus the risk of spoilage, the main factor seems to be the wines themselves, some being much more permissive to B. bruxellensis development than others.

Influence of agrophotovoltaic on vine and must in a cool climate

The current energy crisis means that interest in agrophotovoltaics has increased significantly. The reason behind this is that the system aims to combine agricultural production with energy production. During the three-year period from 2020 to 2022, the effects of photovoltaic panels on the vine, the yield and the quality of the must were studied in Walenstadt in northern Switzerland, an area with a cool, humid climate. 65 Pinot noir vines were planted in the 160m2 study area. Because of the large edge effects, only 3 repetitions with 4 vines each could be created. A significantly lower leaf infestation by Plasmopara viticola was observed among the panels in each of the three years.