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…

VOLTAMETRIC PROFILING OF RED WINE COMPOSITION DURING MACERATION: A STUDY ON FOUR GRAPE VARIETIES

During red wine vinification, maceration allows the must, and consequently the wine, to be enriched with several compounds that contribute to the creation of the typical organoleptic characteristics of red wines. Among these, extraction of polyphenols (PPs) during maceration is a major process of enological interest. The purpose of this study was the evaluate the suitability of a rapid analytical approach based in linear sweep voltammetry to monitor PPs extraction during vinification.

WHICH IMPACT FOR PROANTHOCYANIDIC TANNINS ON RED WINE FRUITY AROMA? SENSORY AND PHYSICOCHEMICAL APPROACHES

Previous research on the fruity character of red wines highlighted the role of esters. Literature provides evidence that, besides these esters, other compounds that are not necessarily volatiles may have an important impact on the overall aroma of wine, contributing to a modulation of its global aromatic expression. The goal of this work was to assess the olfactory consequences of a mixture between esters and proanthocyanidic tannins, through sensory and physico-chemical approaches.
Sensory analysis of numerous aromatic reconstitutions, including triangular tests, detection thresholds, and sensory profiles, were conducted in order to evaluate the sensory impact of tannins on red wine esters perception.

REVEALING THE ORIGIN OF BORDEAUX WINES WITH RAW 1D-CHROMATOGRAMS

Understanding the composition of wine and how it is influenced by climate or wine-making practices is a challenging issue. Two approaches are typically used to explore this issue. The first approach uses chemical
fingerprints, which require advanced tools such as high-resolution mass spectrometry and multidimensional chromatography. The second approach is the targeted method, which relies on the widely available 1-D GC/MS, but involves integrating the areas under a few peaks which ends up using only a small fraction of the chromatogram.

MONOSACCHARIDE COMPOSITION AND POLYSACCHARIDE FAMILIES OF LYOPHILISED EXTRACTS OBTAINED FROM POMACES OF DIFFERENT WHITE GRAPE VARIETIES

The recovery of bioactive compounds from grape and wine by-products is currently an important and necessary objective for sustainability. Grape pomace is one of the main by-products and is a rich source of some bioactive compounds such as polyphenols, polysaccharides, fatty acids, minerals and seed oil. Polysaccharides contained in the grape cell wall can be rhamnogalacturonans type II (RG-II), polysaccharides rich in arabinose and galactose (PRAG), mannoproteins (MP), homogalacturonans (HG) and non pectic polysaccharides (NPP).

FLOW CYTOMETRY, A POWERFUL AND SUSTAINABLE METHOD WITH MULTIPLE APPLICATIONS IN ENOLOGY

Flow cytometry (FCM) is a powerful technique allowing the detection, characterization and quantification of microbial populations in different fields of application (medical environment, food industry, enology, etc.). Depending on the fluorescent markers and specific probes used, FCM provides information on the physiological state of the cell and allows the quantification of a microorganism of interest within a mixed population. For 15 years, the enological sector has shown growing interest in this technique, which is now used to determine the populations present (of interest or spoilage) and the physiological state of microorganisms at the different stages of winemaking.