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…

EVIDENCE OF THE INTERACTION OF ULTRASOUND AND ASPERGILLOPEPSINS I ON UNSTABLE GRAPE PROTEINS

Most of the effects of ultrasound (US) result from the collapse of bubbles due to cavitation. The shockwave produced is associated with shear forces, along with high localised temperatures and pressures. However, the high-speed stream, radical species formation, and heat generated during sonication may also affect the stability of some enzymes and proteins, depending on their chemical structure. Recently, Ce-lotti et al. (2021) reported the effects of US on protein stability in wines. To investigate this further, the effect of temperature (40°C and 70°C; 60s), sonication (20 kHz and 100 % amplitude, for 20s and 60s, leading to the same temperatures as above, respectively), in combination with Aspergillopepsins I (AP-I) supplementation (100 μg/L), was studied on unstable protein concentration (TLPs and chitinases) using HPLC with an UV–Vis detector in a TLPs-supplemented model system and in an unstable white wine.

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.

EUGENOL AS QUALITY MARKER OF WINES AND SPIRITS FROM HYBRID VINES: IMPACT OF DIFFERENT WINEMAKING AND DISTILLATION PROCESSES

Eugenol, widely spread in various plants notably cloves, basil and bay, was identified too in wines from hybrid grapes without contact with oak wood. This aromatic molecule presents a strong spicy note of clove and also antifongic properties. Eugenol was described as an endogenous compound of Baco blanc, from the grapes to the spirits of Armagnac area. Moreover, this compound is a chemical marker of Baco blanc products quality.
Influences of harvest time and different winemaking processes (settling, use of enzymatic preparations, lees content and stock time before distillation) on Baco blanc wine eugenol contents were explored using a two-levels full factorial Design of Experiments (DoEs).

CONSENSUS AND SENSORY DOMINANCE ARE DEPENDENT ON QUALITY CONCEPT DEFINITIONS

The definition of the term “quality” in sensory evaluation of food products does not seem to be consensual. Descriptive or liking methods are generally used to differentiate between wines (Lawless et al., 1997). Nevertheless, quality evaluation of a product such as wine can also relate to emotional aspects. As exposed by Costell (2002), product quality is defined as an integrated impression, like acceptability, pleasure, or emotional experiences during tasting. According to the ‘modality appropriateness’ hypothesis which predicts that wine tasters weigh the most suitable sensory inputs for a specific assess- ment (Freides, 1974; Welch & Warren, 1980), the nature of the quality definitions may modulate sensory influences.

IMPACT OF THE WINES’ QUALITY ON THE WINE DISTILLATES’ ORGANOLEPTIC PROFILE

Brandy de Jerez (BJ) is a spirit drink made exclusively from spirits and wine distillates and is characterized by the use of casks for aging that previously contained Sherries. The quality and sensory complexity of BJ depend on the raw materials and some factors: grape variety, conditions during processing the wine and its distillation, as well as the aging in the cask. Therefore, the original compounds of the grapes from which it comes are of great interest (1 y 2) being in most cases the Airén variety. Their relationship with the quality of the musts and the wines obtained from them has been studied (3) and varies each year of harvest depending on the weather conditions (4).