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…

A NEW SPECIFIC LINEAGE OF OENOCOCCUS OENI IN COGNAC APPELLATION WINES

Oenococcus oeni is the main lactic acid bacteria (LAB) species which conducts the malolactic fermentation (MLF) in wine. During MLF, O. oeni converts malic acid into lactic acid, which modulates wine aroma composition leading to better balanced organoleptic properties. O. oeni is a highly specialized species only detected in environments containing alcohol such as wine, cider or kombucha. Genome analysis of more than 240 strains showed that they form at least 4 main phylogenetic lineages and several sublineages, which are associated with different beverages or types of wines.

YEAST LEES OBTAINED AFTER STARMERELLA BACILLARIS FERMENTATION AS A SOURCE OF POTENTIAL COMPOUNDS TO IMPROVE SUSTAINABILITY IN WINE- MAKING

The yeast residue left over after wine-making, known as wine yeast lees, is a source of various compounds that are of interest for wine and food industry. In winemaking, yeast-derived glycocompounds and proteins represent an example of circular economy approach since they have been proven to reduce the need for bentonite and animal-based fining agents. This leads to a reduced environmental impact in the stabilization and fining processes in winemaking. (de Iseppi et al., 2020, 2021).

‘TROPICAL’ POLYFUNCTIONAL THIOLS AND THEIR ROLE IN AUSTRALIAN RED WINES

Following anecdotal evidence of unwanted ‘tropical’ character in red wines resulting from vineyard interventions and a subsequent yeast trial observing higher ‘red fruit’ character correlated with higher thiol concentrations, the role of polyfunctional thiols in commercial Australian red wines was investigated.
First, trials into the known tropical thiol modulation technique of foliar applications of sulfur and urea were conducted in parallel on Chardonnay and Shiraz.1 The Chardonnay wines showed expected results with elevated concentrations of 3-sulfanylhexanol (3-SH) and 3-sulfanylhexyl acetate (3-SHA), whereas the Shiraz wines lacked 3-SHA. Furthermore, the Shiraz wines were described as ‘drain’ (known as ‘reductive’ aroma character) during sensory evaluation although they did not contain thiols traditionally associated with ‘reductive’ thiols (H2S, methanethiol etc.).

UNRAVELING THE CHEMICAL MECHANISM OF MND FORMATION IN RED WINE DURING BOTTLE AGING : IDENTIFICATION OF A NEW GLUCOSYLATED HYDROXYKETONE PRO-PRECURSOR

During bottle aging, the development of wine aroma through low and gradual oxygen exposure is often positive in red wines, but can be unfavorable in many cases, resulting in a rapid loss of fresh, fruity flavors. Prematurely aged wines are marked by intense prune and fig aromatic nuances that dominate the desirable bouquet achieved through aging (Pons et al., 2013). This aromatic defect, in part, is caused by the presence of 3-methyl-2,4-nonanedione (MND). MND content was shown to be lower in nonoxidized red wines and higher in oxidized red wines, which systematically exceeds the odor detection threshold (62 ng/L).

VOLATILE, PHENOLIC AND COLORIMETRIC CHARACTERIZATION OF THREE DIFFERENT LAMBRUSCO APPELLATIONS

Lambrusco is a commercially successful sparkling red and rosé wine. With 13.06 million litres sold in 2021 was the second best-selling Italian wine after Chianti. According to National Catalogue of Vine Varieties there are thirteen Lambrusco Varieties with which to date are produced seven PDO wines. Among these, “Lambrusco Salamino di Santa Croce”, “Lambrusco Grasparossa di Castelvetro” and “Lambrusco di Sorbara” are the only ones that can be considered mono-varietal appellations, all located in Modena area. The PDOs contemplate the possibility of producing wines by secondary fermentation either in tank (Charmat method), or in bottle (Classico method). Sur lie is a third method commonly employed for Lambrusco, similar to the Classico method, from which differs for the absence of disgorgement.