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…

IDENTIFICATION OF NEW RESVERATROL DERIVATIVES FORMED IN RED WINE AND THEIR BIOLOGICAL PROPERTIES

Stilbenes are natural bioactive polyphenols produced by grapevine. Recently, we have reviewed the na- tural presence of these compounds in wines [1]. This study showed that the resveratrol and its glycoside, the piceid, are the most abundant stilbenes in wines. Resveratrol is a well-known stilbene with a wide range of biological activities. Due to its specific structure, resveratrol can be oxidized in wines to form various derivatives including oligomers [2]. In this study, we investigate the resveratrol and piceid transformation in wines.

METHYL SALICYLATE: A TRENDY COMPOUND MARKER OF ZELEN, A UNIQUE SLOVENIAN VARIETY

The wine market interest for autochthonous varieties, particularly from less known wine regions, has significantly raised in the past few years. In that context, Slovenia, a small country from central Europe with a long winemaking tradition, is getting more and more attention, particularly through its range of unique regional varieties. Among them, Zelen, meaning “green” in Slovene, can only be found in the Vipava valley region, located on the western side of the country, near the border with Italy. When they are young, Zelen wines display very singular aromas reminiscent of rosemary, sage and white fruit. Despite its uniqueness, Zelen wine aromatic typicality is poorly documented in the literature.

ADDITION OF OAK WOOD ALTERNATIVE PRODUCTS: QUALITATIVE AND SENSORIAL EFFECTS FOR A WHITE WINE OF ALIGOTE

Wines matured in contact with wood are extremely popular with consumers all over the world. Oak wood allows the organoleptic characteristics of wine to be modified. Wines are enriched with volatile and non-volatile compounds extracted from the wood. The aromas extracted from oak wood contribute to the construction of the wine’s aromatic profile and the main polyphenols extracted can modify taste perceptions such as astringency and bitterness. All the compounds extracted from the wood thus contribute to the balance and quality of the wines.

UNEXPECTED PRODUCTION OF DMS POTENTIAL DURING ALCOOLIC FERMENTATION FROM MODEL CHAMPAGNE-LIKE MUSTS

The overall quality of aged wines is in part due to the development of complex aromas over a long period (1.) The apparition of this aromatic complexity depends on multiple chemical reactions that include the liberation of odorous compounds from non-odorous precursors. One example of this phenomenon is found in dimethyl sulphide (DMS) which, with its characteristic odor truffle, is a known contributor to the bouquet of premium aged wine bouquet (1). DMS supposedly accumulates during the ten first years of ageing thanks to the hydrolysis of its precursor dimethylsulfoniopropionate (DMSp.) DMSp is a possible secondary by-product from the degradation of S-methylmethionine (SMM), an amino acid iden- tified in grapes (2), which can be metabolized by yeast during alcoholic fermentation.

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.