At present, the geographical origin of extra virgin olive oils can be ensured by documented traceability, although chemical analysis may add information that is useful for possible confirmation. This preliminary study investigated the effectiveness of flash gas chromatography electronic nose and multivariate data analysis to perform rapid screening of commercial extra virgin olive oils characterized by a different geographical origin declared in the label. A comparison with solid phase micro extraction coupled to gas chromatography mass spectrometry was also performed. The new method is suitable to verify the geographic origin of extra virgin olive oils based on principal components analysis and discriminant analysis applied to the volatile profile of the headspace as a fingerprint. The selected variables were suitable in discriminating between "100% Italian" and "non-100% Italian" oils. Partial least squares discriminant analysis also allowed prediction of the degree of membership of unknown samples to the classes examined.
Sensory evaluation, carried out by panel tests, is essential for quality classification of virgin olive oils (VOOs), but is time consuming and costly when many samples need to be assessed; sensory evaluation could be assisted by the application of screening methods. Rapid instrumental methods based on the analysis of volatile molecules might be considered interesting to assist the panel test through fast pre-classification of samples with a known level of probability, thus increasing the efficiency of quality control. With this objective, a headspace gas chromatography-ion mobility spectrometer (HS-GC-IMS) was used to analyze 198 commercial VOOs (extra virgin, virgin and lampante) by a semi-targeted approach. Different partial least squares-discriminant analysis (PLS-DA) chemometric models were then built by data matrices composed of 15 volatile compounds, which were previously selected as markers: a first approach was proposed to classify samples according to their quality grade and a second based on the presence of sensory defects. The performance (intra-day and inter-day repeatability, linearity) of the method was evaluated. The average percentages of correctly classified samples obtained from the two models were satisfactory, namely 77% (prediction of the quality grades) and 64% (prediction of the presence of three defects) in external validation, thus demonstrating that this easy-to-use screening instrumental approach is promising to support the work carried out by panel tests.
A set of 334 commercial virgin olive oil (VOO) samples were evaluated by six sensory panels during the H2020 OLEUM project. Sensory data were elaborated with two main objectives: (i) to classify and characterize samples in order to use them for possible correlations with physical–chemical data and (ii) to monitor and improve the performance of panels. After revision of the IOC guidelines in 2018, this work represents the first published attempt to verify some of the recommended quality control tools to increase harmonization among panels. Specifically, a new “decision tree” scheme was developed, and some IOC quality control procedures were applied. The adoption of these tools allowed for reliable classification of 289 of 334 VOOs; for the remaining 45, misalignments between panels of first (on the category, 21 cases) or second type (on the main perceived defect, 24 cases) occurred. In these cases, a “formative reassessment” was necessary. At the end, 329 of 334 VOOs (98.5%) were classified, thus confirming the effectiveness of this approach to achieve a better proficiency. The panels showed good performance, but the need to adopt new reference materials that are stable and reproducible to improve the panel’s skills and agreement also emerged.
This research aims to develop a classification model based on untargeted elaboration of volatile fraction fingerprints of virgin olive oils (n = 331) analyzed by flash gas chromatography to predict the commercial category of samples (extra virgin olive oil, EVOO; virgin olive oil, VOO; lampante olive oil, LOO). The raw data related to volatile profiles were considered as independent variables, while the quality grades provided by sensory assessment were defined as a reference parameter. This data matrix was elaborated using the linear technique partial least squares-discriminant analysis (PLS-DA), applying, in sequence, two sequential classification models with two categories (EVOO vs. no-EVOO followed by VOO vs. LOO and LOO vs. no-LOO followed by VOO vs. EVOO). The results from this large set of samples provide satisfactory percentages of correctly classified samples, ranging from 72% to 85%, in external validation. This confirms the reliability of this approach in rapid screening of quality grades and that it represents a valid solution for supporting sensory panels, increasing the efficiency of the controls, and also applicable to the industrial sector.
The commercial category of virgin olive oil is currently assigned on the basis of chemical-physical and sensory parameters following official methods. Considering the limited number of samples that can be analysed daily by a sensory panel, an instrumental screening tool could be supportive by reducing the assessors’ workload and improving their performance. The present work aims to in-house validate a screening strategy consisting of two sequential binary partial least squares-discriminant analysis (PLS-DA) models that was suggested to be successful in a proof-of-concept study. This approach is based on the volatile fraction fingerprint obtained by HS-SPME–GC–MS from more than 300 virgin olive oils from two crop seasons graded by six different sensory panels into extra virgin, virgin or lampante categories. Uncertainty ranges were set for the binary classification models according to sensitivity and specificity by means of receiver operating characteristics (ROC) curves, aiming to identify boundary samples. Thereby, performing the screening approach, only the virgin olive oils classified as uncertain (23.3%) would be assessed by a sensory panel, while the rest would be directly classified into a given commercial category (78.9% of correct classification). The sensory panel’s workload would be reduced to less than one-third of the samples. A highly reliable classification of samples would be achieved (84.0%) by combining the proposed screening tool with the reference method (panel test) for the assessment of uncertain samples.
This study aims at evaluating the effect of a phenol-rich extract obtained from the concentration and purification of olive mill wastewaters (added at a ratio of 87.5 and 175 mg of phenols/kg meat) on the stability and sensory quality of beef hamburgers packed under modified atmosphere and stored under alternating exposure to fluorescent light at 4 ± 2 °C for 9 days. The hamburgers were sampled at different times (0, 6, and 9 days) and grilled at 200 °C. After 9 days, more than 56% of the added phenols in the raw burgers and more than 20% the grilled ones were retained. The results show that both concentrations of phenolic extract proved to effectively reduce primary and secondary lipid oxidation, as well as cholesterol oxidation products (COPs), during the shelf-life of raw hamburgers. Peroxide value, thiobarbituric acid reactive substances, and total COPs were up to 1.4-, 4.5-, and 8.8-fold lower in phenol-enriched raw hamburgers, respectively, than in the control samples; a similar trend was noted also in phenol-enriched cooked hamburgers (1.3-, 5.7-, and 4-fold lower). The sensory analysis also confirmed the effectiveness of the addition of phenolic extract, resulting in a positive effect on the red color intensity (raw product) and thus reducing browning during storage.