Using 1H-NMR combined with chemometrics to discriminate the effect of different cuts and toasting of woods used for grape pomace distillate ageing

Abstract

The purpose of this research study is to consider new solutions for distillate ageing, in alternative to conventional oak chips or barrels in particular sliced wood and peeled wood were compared to oak cubes, normally employed during both wine and distillate ageing. All three formats have been toasted using a “in lab” protocol at three different level of intensity: strongly toasted, lightly toasted and not toasted.
NMR spectroscopy was used to assess the differences, in and the chemical fingerprint among experimental distillates, aged using woods with different cuts and toasting levels.
NMR spectrometry is widely used in food analysis for metabolomic studies and for the evaluation of samples that have undergone different treatments. NMR allows to obtain a complex fingerprint spectrum characterised by the chemical species of the samples. The advantages of high resolution 1H-NMR are absolute reproducibility and laboratory-to-laboratory transferability, compared to other method currently used in food analysis. The region between 11 and 6 ppm of 1H-NMR spectra was chosen focussing on the range where main structural differences related to xylovolatile compounds, namely phenols, aldehydes and aromatic groups were present.
The obtained 1H-NMR data sets were firstly analysed by chemometric multivariate unsupervised methods, that showed a good separation between the control sample (i.e. distillates aged without oak) and all other samples, as well as between the different sample groups. In particular, principal components analysis (PCA), Anova-Simultaneous components analysis (ASCA) and hierarchical cluster analysis (HCA) were calculated and compared. This approach showed that samples refined with strongly, lightly or not toasted wood present a different molecular profile. A group separation was observed based on the wood cut type (i.e. sliced, peeled or cubes). Moreover, a non-negligible effect of the interaction between cut type and the toasting level was noticed.
Hence, the results confirmed the ageing process, that affects the chemical profile of grape pomace distillates, can be effectively monitored by NMR analysis. This provides a promising tool for distinguishing the different ageing conditions of spirits and assessing their quality