Grappa is a traditional Italian grape marc spirit protected by geographical indication. Monovarietal Grappa, from a single grape variety, exhibits distinctive compositional and sensory characteristics linked to the selected raw materials, including denominations such as Grappa di Barolo. Rapid screening methods are essential for product authentication. This study analyzed the volatile fingerprints of 45 Grappa samples from four grape varieties (Muscat, Prosecco, Barolo, Brunello) using Flash GC. Multivariate linear (PCA and PLS-DA) and non-linear (C-SVM) techniques were applied to different data representations including full chromatographic profiles, selected chromatographic regions and peak-area data to determine which representation offered the highest discriminant power. Comparable classification results were obtained using both PLS-DA and SVM models, reporting overall accuracy ranging from 77.8 to 84.1% in cross-validation. Tentative identification of discriminating compounds was also performed. The results suggest the potential of Flash GC and chemometrics as a rapid screening tool to discriminate monovarietal Grappa.
The present study investigated the consumer response to pasta formulated with hemp, seaweed, insect and pea flours or powders among the Italian population, given the urgent need to identify and utilise alternative, sustainable protein sources. To this end, a structured questionnaire was administered to 470 participants to assess their eating habits, their familiarity with high-protein products, and how nutritional and environmental information influences their willingness to try (WTT) and willingness to buy (WTB) the herein-evaluated pastas. Attitudes such as food neophobia, interest in health and sustainability of food consumption were also examined using psychometric scales. The findings indicated higher WTT and WTB values for pea protein pasta, which were significantly and positively influenced by nutritional information. The study further demonstrated a differential behavioural pattern: participants with lower food neophobia scores exhibited a greater propensity to adopt novel protein sources, whereas highly neophobic individuals appeared less responsive to informational treatments. In addition, a cluster analysis identified two distinct consumer segments differing markedly in their WTT and WTB. Among the examined variables, low food neophobia, rather than consumer predisposition towards the health-related attributes of food or their focus on environmental sustainability, was consistently associated with greater WTT and WTB for alternative protein sources. The promotion of foodstuffs containing alternative protein sources, particularly those that are unfamiliar or associated with psychological barriers identified in previous literature, such as food neophobia and food disgust, may benefit from a combination of nutritional and environmental messaging to counterbalance these barriers.
In recent decades, the concept of food pairing has gained importance across various aspects of gastronomic science. Flavoured oils serve as an excellent case for exploring food pairing with specific culinary preparations. Simultaneously, as consumers increasingly prioritize sustainability in food production, the search for ingredients that are both sustainable and appealing has become essential for both producers and consumers. This study investigates the willingness to try (WTT) and buy (WTB) three oils flavoured with by-products from food production and explores consumers' preferences toward pairing these oils with different culinary preparations, all within a virtual context.The dataset was analysed through Cochran's Q test to examine CATA (Check-All-That-Apply) data, with the objective of identifying the culinary preparations most frequently associated with each of the three oil types. Subsequently, six OLS (Ordinary Least Squares) models were implemented - two for each oil: one for WTT and one for WTB - to determine the drivers influencing each willingness. The exploratory survey, conducted with 333 Italian consumers, revealed key insights: first, how consumers pair these oils with various culinary preparations, offering valuable directions for practical sensory analysis, and second, highlight the factors that most influence WTT and WTB oils flavoured with agri-food by-products.
Consumers are increasingly attracted to innovative, gourmand, and sustainable food products. This has led to a growing interest in flavored olive oils through co-milling processing. This study explores the production and characterization of flavored olive oils obtained by co-milling olives with orange pomace, black pepper, and hemp seeds, aiming to enhance their sensory and compositional properties while promoting sustainability through the valorization of agri-food by-products. The flavored olive oils and their control samples were analyzed for free acidity, tocopherols, phenolic compounds, volatiles, and sensory profiles. The flavored oils exhibited an acceptable hydrolytic state and peculiar sensory notes, depending on the ingredients used, as well as enhanced compositional qualities. This research highlights the potential of using oranges and hemp by-products in flavored oil production, offering an innovative approach to reducing food waste, with the possibility of future industrial applications.
The changes in monovarietal extra virgin olive oils (EVOOs), produced with olives grown under different agronomic conditions, were investigated by targeted and untargeted analytical approaches. Specifically, volatile molecules were monitored in oils just produced and stored for 6 and 12 months with two different packaging solutions. The targeted SPME-GC–MS method showed an increase in volatile markers of lipid oxidation. Moreover, more rapid analytical approaches, namely targeted HS-GC–IMS and untargeted FGC, were used to investigate volatile organic compounds (VOCs). These chromatographic methods, respectively, returned heatmaps and fingerprint profiles that were elaborated on by multivariate analysis. Exploratory principal component analysis performed on the data from VOCs allowed the clustering of samples based on the storage time. The quality of samples was also determined by a panel test. Furthermore, this study employed previously built models using partial least squares discriminant analysis to confirm the sensory classification of the stored samples. Based on these predictive models, all samples were confirmed as EVOO, except for one categorized as virgin (rancid according to the panel test). This classification was further supported by the SPME-GC–MS analysis, which revealed higher concentrations of lipid oxidation markers in this specific sample, in particular the (E)-2-heptenal reached a concentration twenty times higher than its odor threshold. In addition, five oils were inconsistently classified by the models and considered at risk of downgrading the commercial category after 12 months of storage.
Using a multi-analytical approach, this investigation characterized Parmigiano Reggiano PDO cheese produced with milk from dairy cows fed different diets. Ten samples of Parmigiano Reggiano PDO cheese, aged for 24 months, were produced with milk from dairy cows fed only dry hay (P-DH; N = 6) or a diet with part of the dry hay replaced with fresh herbage (P-FF; N = 4). Instrumental (Flash GC-FID) analysis of the volatile fraction, image analyses, and sensory quantitative descriptive analysis (QDA®) were carried out. The Parmigiano Reggiano cheese belonging to the P-FF group showed a higher intensity of yellow than P-DH for both sensory and image analyses. Regarding the volatile profiles, no differences were observed related to the two experimental groups, while sensory analyses allowed for some discrimination, in particular color and aroma attributes. Instrumental and sensory characterization can be used to obtain a unique analytical profile for Parmigiano Reggiano PDO cheeses produced with milk from dairy cows fed different forage sources and help to define the quality and authenticity of this typical high-value food product.
1H NMR fingerprinting of virgin olive oils (VOOs) and a collection of binary classification models arranged in a decision tree are presented as a stepwise strategy to determine the geographical origin of a VOO at four levels, i.e. provenance from an EU member state or outside the EU, country and region of origin, and compliance with a geographical indication scheme. This approach supports current EU regulation that makes labelling of the geographical origin mandatory for olive oil. Currently, official methods for its control are still lacking. Partial least squares discriminant analysis (PLS-DA) and random forest for classification afforded robust and stable binary classification models to verify the geographical origin of VOOs; however, the former outperformed the latter in terms of accuracy and robustness. The prediction abilities of the best binary PLS-DA model for each case study were between 80% and 100% for both classes in cross-validation and in external validation. The satisfactory results achieved for the verification of the geographical origin of VOOs, together with those of our previous studies on the discrimination of olive oil categories, the detection of olive oils blended with vegetable oils (Alonso-Salces et al., 2022), and the determination of the stability, freshness, storage time and conditions, and olive oil best-before date (Alonso-Salces et al., 2021), confirm that a single 1H NMR analysis of an olive oil sample can provide useful information to control several EU regulations related to olive oil marketing standards (Regulation (EU) 2022/2104 and Regulation (EU) 2024/1143).
In recent years, different gas-chromatographic methods based on the determination of volatile compounds, combined with chemometrics, have been proposed as methods to support the olive oil Panel test in classifying samples into commercial categories (EV, extra virgin olive oil; V, virgin olive oil; L, lampante olive oil). A valid strategy is to merge the outcomes of different analytical sources, applying a data fusion. This approach may be useful to improve the efficiency of prediction and robustness of a model compared to the results obtained by individual screening methods. In this analysis, inputs obtained by HS-GC-IMS and FGC E-nose analyses of 246olive oil samples were elaborated to classify samples according to commercial categories (EV, V, or L). PLSDA models based on three (EV, V, and L) or two classes (EV vs noEV, L vs noL, EV vs V, and L vs V) were developed. Furthermore, two different data fusion strategies (low and mid fusion level) were tested. In the lowlevel fusion, data from the two sources were concatenated directly, while in the mid-level fusion, features extracted separately from each source were combined into a common data matrix. Regardless of the single data set or data fusion approach, the strategy based on two class PLS-DA models showed the best results in which the percentages obtained in test set validation (TSV) ranged from 77.8% to 86.7% (FGC E-nose) and from 75% to 89.6% (HS-GC-IMS). A clear increase of the percentage of correctly classified samples was reached adopting the data fusion strategy, especially for class V (low level data fusion: +16.6%; mid level data fusion: +12.5%) and EV (+12.0% for both data fusion levels). Comparing the two strategies, mid level data fusion showed the most effective performance for both techniques, HS-GC-IMS (8.3 +/- 6.4%) and FCG-E-nose (8.7 +/- 4.8%), compared to the low fusion level, in which average percentage increases of 5.3 +/- 2.7% and 6.4 +/- 5.6% were reported with respect to the results of HS-GC-IMS and FGC E-nose models, respectively. The highest increases were achieved for L vs V models for both data fusion strategies. These promising results suggest that the data fusion approach can be an option to enhance the predictive efficiency in classifying olive oil samples into three commercial categories, providing a more reliable method to support the Panel test compared to the use of the single techniques.
Tomato pomace (TP) is an underutilized source of bioactive compounds with potential application in the food sector. A factorial experiment was designed to compare three culinary techniques, Thermomix®, Roner®, and traditional pan-frying, for the preparation of tomato sauces, enriched or not with TP, applying two temperatures and two cooking times. A multivariate analysis was performed on all the results obtained for the metabolites. The addition of TP significantly increased the content of bioactive compounds, especially phenolic compounds. OPLS-DA models were generated using cooking technique, temperature, and time as discriminant factors. The cooking technique had a greater effect on the phenolic content than cooking temperature or time. Thermomix® released bioactive compounds from the tomato into the sauce to a similar extent as pan-frying. Roner® proved to be effective in preserving the volatile fraction of the sauce. The Thermomix® significantly increased the amount of bioactive compounds, while the Roner® increased the volatile compounds.
Extra virgin olive oil (EVOO) quality and composition are mainly affected by genetics, agronomic and technological parameters, undergoing further modifications during storage. In this work, a chemometric approach was applied to study the impact of olive maturity, malaxation time/temperature, and oil storage on the quality and compositional parameters of Arbequina EVOO (basic quality indices, volatile and sensory profiles, contents in phenolic compounds, squalene, vitamin E and fatty acids). Storage emerged as the most influential factor, followed by olive maturity and malaxation temperature, while malaxation time had almost no effect. Storage at room temperature had a significant impact on the phenolic profile and quality parameters, mainly the peroxide value and K270. The determination of K270, an indicator of secondary oxidation products, was relevant to analyze the effect of storage conditions. Volatile compounds and fatty acids were good markers of ripeness, and the volatile profile was highly affected by malaxation temperature.
Olive pomace results from the production of olive oil. Even if olive pomace represents a potential environmental problem, it contains phenolic compounds, which are widely recognized for their beneficial properties for human health. In this study, an innovative and sustainable technological approach to extract phenolic compounds from fresh olive pomace, based on food-grade solvent instead of those usually adopted, is investigated. Characterization and shelf-life evaluation of the hydroalcoholic extracts obtained from the procedure developed for different industrial purposes were also carried out. The phenolic fractions of the different samples were studied with the Folin–Ciocâlteu method to quantify that the total reducing molecules and HPLC-MS/MS analysis was used to define the profile through the identification and quantification of 42 compounds, belonging to five chemical families. Regarding shelf-life, the hydroalcoholic extract showed no significant reduction in phenolic content, for both instrumental evaluations, retaining most of the phenolic compounds present in the raw material; negative attributes were not perceived by sensory evaluation. Thus, these lab-scale results can be the starting point to develop a procedure that is suitable for a real olive mill, representing a valorization strategy in a circular economy and the perspective of new business models.
This study aimed to investigate consumer sensory profiles and liking of Parmigiano Reggiano PDO cheese produced with milk from cows reared indoors and fed with different forage sources, i.e., dry hay and fresh forage. Two cheese samples were tested by 119 Italian subjects, following a protocol that included a Check-All-That-Apply method to assess the sensory profile, a Just-About-Right scale to evaluate the adequacy of attributes, and questions on liking (9-point hedonic scale). A questionnaire related to personal information and consumption habits was also submitted. The color of the two samples, based on image analysis, was different: the sample produced with milk from the dairy cows fed fresh forage had a higher intensity of yellow than the other; they were also described differently (p ≤ 0.05) by participants in the consumer test. Indeed, Parmigiano Reggiano produced with milk from the cows that were fed dry hay was mainly characterized by a "fresh milk" and "solubility", while the sample produced with milk from cows fed fresh forage was described as "yellow", "seasoned", "pungent", and with a "cheese crust" flavor. Even if no significant differences were observed between the two samples in terms of liking (p ≤ 0.05), the attribute "graininess" showed a great impact on liking ratings together with "yellow" (p ≤ 0.05), apparently corresponding to a specific expectation regarding the intensity of these attributes. Data were also analyzed according to the gender of consumers, highlighting that for women, the adequacy of "fresh milk", "sweet", and "graininess" greatly impacted liking for the cheese from cows fed dry hay.
The disposal of waste from widely consumed foods, such as tomatoes, poses a considerable challenge for the agro-industry. Tomato pomace (TP), a by-product of tomato processing consisting of peels and seeds, is an underutilized source of bioactive compounds with potential application in the food sector. In this work, a factorial experiment was designed to compare three culinary techniques, Thermomix® and Roner® food processing and traditional pan-frying, for the preparation of tomato sauces, enriched or not with TP, applying two temperatures and two cooking times. A multivariate analysis was performed on all the results obtained for the studied metabolites. The addition of TP significantly increased the content of bioactive compounds in the tomato sauce, especially phenolic compounds. OPLS-DA models were generated, using cooking technique, temperature, and time as discriminant factors. The culinary technique had a greater effect on the phenolic content than cooking temperature or duration time. During processing in the Thermomix®, but not the Roner®, bioactive components were released from tomato into the sauce to a similar extent as traditional pan-frying. Although no significant increase in bioactive compounds was found when using the Roner®, this technique proved effective in preserving the volatile fraction of the sauce. The two new cooking home technologies evaluated, comparing with the classical pan frying, have different effect on the tomato sauce preparation; while the Thermomix ®, increased significatively the amount of bioactive compounds, the Roner® increased the amount of volatile compounds.
Halyomorpha halys is an insect native to eastern Asia, which in recent years has spread widely throughout Europe and is able to cause extensive damage to agricultural production. The damage is mainly associated with the trophic activity that can take place in various plant organs. H. halys damage to agricultural production can affect olive production, quantitatively reducing production and damaging the quality of the oils produced. In the present work, the damage caused on the olives of "Dritta" and "Leccino" cultivars and the effects on the chemical, physical-chemical, and sensory characteristics of the oils obtained from the damaged olives were evaluated. The results showed that oils obtained from infested olives had lower quality. There was a statistically significant reduction in the content of phenols, tocopherols, bioactive antioxidant substances, and positive descriptors (fruity, bitter, pungent) in the organoleptic taste. Moreover, the oils obtained from the damaged olives showed organoleptic defects, mainly mold, compared with oils obtained from healthy drupes.
A particular aspect of quality control of virgin olive oil (VOO) is the mandatory application, together with chemical and instrumental determinations, of a standardized and official method for sensory assessment. The latter, known as Panel test, is carried out by trained assessors and contributes to the classification of VOOs into three commercial categories (extra virgin, virgin, and lampante). One drawback of this method is related to the large number of samples to be analyzed, compared to the work capacity of a sensory panel, especially during the selection for purchase by companies that blend and market virgin oils and the quality control conducted by the authorities to verify the declared commercial category. For this reason, it is helpful to develop and validate robust and rapid screening methods, based on volatile fingerprints, to preclassify each sample into one of the three commercial categories. Considering the strict relation between volatile compounds and the main sensory attributes (fruity and defects), a gas-chromatographic volatile fingerprint can be the right choice. In this paper, the comparison of two emerging techniques, namely, headspace-gas chromatography-ion mobility spectrometry (HS-GC-IMS) and flash-gas chromatography (FGC), applied on a sample set of 49 VOOs, using calibrations previously built with a larger number of samples, is presented. The number of correctly classified samples, with respect to the commercial category determined by the Panel test, was satisfactory and comparable (92% for HS-GC-IMS, and 94% for FGC), confirming the effectiveness of both methods and the robustness of the predictive models.Practical Applications: The demand for rapid screening tools to reduce the number of samples to be assessed by the Panel test has increased in recent years. The validation of robust models and their joint adoption by companies that market VOOs as well as official control bodies could reduce nonconformities and increase the batches of VOO being controlled, thus better protecting the consumer. Therefore, it is desirable to have different tools available to analyze volatile compounds, together with the associated calibration models, along with detailed instructions for their application, to have different alternatives that suit the equipment of individual laboratories. Rapid screening methods can support sensory analysis by preclassifying samples to prioritize and/or reduce the number of VOOs to be assessed by the Panel test. image
A “green breakthough” at the table due to consumer demand for healthy and sustainable foods, which aligns with the typical Mediterranean diet, has recently led to an increase in the consumption of products such as extra virgin olive oil. In fact, Italian olive cultivation, which contributes an average of 15% of world production, has seen the production of extra virgin olive oil with a value of exports that have doubled in the last 20 years. In this context, the olive oil sector of the Emilia-Romagna region (Italy), and in particular the PDO Brisighella, could achieve greater success with consumers by proposing a product obtained through sustainable agriculture that enhances the content of bioactive compounds. For these reasons, in this study, different agronomic variables are investigated in order to optimize the presence of bioactive components in extra virgin olive oil made from monovarietal Nostrana di Brisighella, namely phenolic and positive volatile compounds, thus naturally enriching this product both from health and sensory points of view. The study focuses on the volatile and phenolic fractions (derivatives of hydroxytyrosol and tyrosol) of olive oil and the positive sensory attributes (fruity, bitter and pungent) that are known to be associated with these molecules. The phenolic content is of particular interest due to the potential to support health claims. Extra virgin olive oil samples were produced from olives of the Nostrana di Brisighella cultivar; fruits were obtained through integrated pest management or organic farming and picked at four increasing indices of maturity, corresponding to four successive weeks of harvesting. These agronomic variables influenced the compositional and sensory characteristics of the extra virgin olive oils assessed, highlighting differences that likely derive from the effect of the agronomic system used, i.e., integrated pest management or organic farming.
The organoleptic assessment (Panel test) is the only procedure within the official methods for determining the quality of virgin olive oils that involves an expert panel. There is an urgent need for analytical methodology that can reliably measure volatile compounds in virgin olive oils that is capable of supporting and anticipating the official Panel test. For this reason, a new method based on solid‐phase microextraction–gas chromatography with the choice of two possible detectors (FID or MS) was subjected to a large international interlaboratory validation study. The study involved a two‐stage process: first, a pretrial phase in which 7 participants were exposed to the method for the first time to identify any initial problems with the methodology; then, a formal validation stage (trial proper), which involved 20 laboratories from Europe, USA, Japan and China. The performance of the different detectors was investigated. While both methods have advantages, the method using FID provided better results for 11 compounds, in terms of reproducibility, compared to MS. This information will allow to implement the method with accurate information of the method performance depending on the detector used. Practical applications: This study provides information from an interlaboratory validation of a method for measuring volatile compounds in virgin olive oils conducted with laboratories (from industry and academia) working in the olive oil sector. The information on the expected analytical errors in the determination of each volatile compound is necessary to apply this method for supporting the official Panel test (sensory analysis). The SPME‐GC‐MS/FID methods proposed in this work can be used for the internal quality control of a company/distributor/quality control laboratory and could also be used in cases of difficult/contradictory organoleptic assessment, or to confirm results from sensory panels in cases of disputes/disagreement (Reg. EU 2022/2105).