Optimising the acquisition conditions of high information quality low-field NMR signals based on a cutting-edge approach applying information theory and Taguchi's experimental designs – Virgin olive oil as an application example

Abstract

Background_: Developing a new spectrometric analytical method based on a fingerprinting approach requires optimisation of the experimental stage, particularly with novel instruments like benchtop low-field NMR spectrometers. To ensure high-quality LF-NMR spectra before developing the multivariate model, an experimental design to optimise instrument conditions is essential. However, difficult-to-control factors may be critical for optimisation. Taguchi methodology addresses these factors to obtain a system robust to variation. This study uses the Taguchi methodology to optimise instrument settings for acquiring high-quality 1H and 13C LF-NMR signals in a short time from virgin olive oil (VOO). Results_: Two experimental trials (for 1H and 13C signals, respectively) were carried out and analysed to find an optimal and robust combination of instrument settings against changes in two difficult-to-control factors: ambient temperature and small deviations of the NMR tube volume (700 ± 50 μL). The responses to be optimised, run time and spectral information quality, were analysed separately and jointly, as some factors showed opposite behaviour in the effect on the responses. Multiple response analysis based on suitable desirability functions yielded a combination of factors resulting in desirability values above 0.8 for 1H LF-NMR signals and almost 1.0 for 13C LF-NMR signals. In addition, a novel approach to assess the information quality of an analytical signal was proposed, addressing a major challenge in analytical chemistry. By applying information theory and calculating information entropy, this approach demonstrated its potential for selecting the highest quality (i.e. most informative) analytical signals. Significance_: The acquisition instrument conditions of LF-NMR were successfully optimised using Taguchi methodology to acquire highly informative 1H and 13C spectra in a minimum run time. The importance lies in the future development of non-targeted analytical applications for VOO quality control. In addition, the innovative use of information entropy to a priori assess the signal quality represents a significant advance and proposes a solution to a long-standing challenge in analytical chemistry.