Geographical Origin Assessment of Extra Virgin Olive Oil via NMR and MS Combined with Chemometrics as Analytical Approaches

Abstract

Geographical origin assessment of extra virgin olive oil (EVOO) is recognised worldwide as raising consumers’ awareness of product authenticity and the need to protect top-quality products. The need for geographical origin assessment is also related to mandatory legislation and/or the obligations of true labelling in some countries. Nevertheless, official methods for such specific authentication of EVOOs are still missing. Among the analytical techniques useful for certification of geographical origin, nuclear magnetic resonance (NMR) and mass spectroscopy (MS), combined with chemometrics, have been widely used. This review considers published works describing the use of these analytical methods, supported by statistical protocols such as multivariate analysis (MVA), for EVOO origin assessment. The research has shown that some specific countries, generally corresponding to the main worldwide producers, are more interested than others in origin assessment and certification. Some specific producers such as Italian EVOO producers may have been focused on this area because of consumers’ interest and/or intrinsic economical value, as testified also by the national concern on the topic. Both NMR- and MS-based approaches represent a mature field where a general validation method for EVOOs geographic origin assessment could be established as a reference recognised procedure.

A review: role of mass spectrometry in the quality and authenticity identification of olive oil

“…It was found that each edible oil had a unique fingerprint profile, which could reveal the difference between OO and other edible oils. Cal o et al (2022), through detailed literature research, showed that mass spectrometry is an effective analytical technique for evaluating the geographical origin of EVOOs. In this article, the applications of mass spectrometry in OO authentication were summarised, and the development direction and trends of mass spectrometry in OO authentication have been prospected.…”

Nuclear magnetic resonance spectroscopy in extra virgin olive oil authentication

“…The analysis of the lipid profile through HPLC with MS detection and through 1 H NMR allowed the identification of new markers, uvaol, and oleanolic acid, the most significant, which distinguish PDO EVOO from family farms to commercially blended EVOO. Calò et al (2022) deeply discussed the use of NMR and MS spectroscopies combined with chemometrics for geographical assessment, highlighting the good performances and usefulness of these two techniques. A development of NMR fingerprint methods in combination with statistical analysis to address the geographical origin issue of EVOOs was reported by Coco et al (2012), who studied 12 authentic olive oils from Italy, Greece, Tunisia, and Spain and 25 commercially available ''Italian olive oils'' in the US market with NMR and PCA.…”

“…Calò et al. (2022) deeply discussed the use of NMR and MS spectroscopies combined with chemometrics for geographical assessment, highlighting the good performances and usefulness of these two techniques. A development of NMR fingerprint methods in combination with statistical analysis to address the geographical origin issue of EVOOs was reported by Coco et al.…”

“…NMR spectroscopy, well known for structure elucidation, is also a powerful tool for food quality control, geographical characterization, and product authentication (Mannina et al., 2012; Piccinonna et al., 2016), and it is a very promising technique, especially if followed by a chemometric approach (Beteinakis et al., 2020). The NMR methodology has numerous advantages, such as no need for time‐consuming sample preparation steps plus high reproducibility and automation (Calò et al., 2022). The major drawback of NMR is its intrinsic sensitivity, which is lower than the sensitivity of other chromatographic and mass‐spectrometry methodologies, even if it can be improved through the application of more elaborate equipment, such as cryoprobes (Pan & Raftery, 2007).…”

Identification of Turkish extra virgin olive oils produced in different regions by using NMR (1H and 13C) and IRMS (13C/12C)

“…Official methods for specific authentication of EVOOs, such as geographic origin assessment, are still lacking today. Among the useful analytical techniques for geographical origin certification and authentication, 1 H and 13 C NMR and IRMS, along with chemometry, are widely used (Calò et al, 2022; Jiménez‐Morillo et al, 2020; Ogrinc et al, 2003). As known EVOOs show significant differences in sensory, nutritional and functional characteristics (aromas, polyphenols, and tocopherols) related to the olive variety, production technology and geographical origin.…”