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Background: Gas chromatography-ion mobility spectrometry (GC-IMS) is a powerful analytical technique which has gained widespread use in a variety of fields. Detecting peaks in GC-IMS data is essential for chemical identification. Topological data analysis (TDA) has the ability to record alterations in topology throughout the entire spectrum of GC-IMS data and retain this data in diagrams known as persistence diagrams. To put it differently, TDA naturally identifies characteristics such as mountains, volcanoes, and their higher-dimensional equivalents within the original data and measures their significance., Results: In the present contribution, a novel approach based on persistent homology (a flagship technique of TDA) is suggested for automatic 2D peak detection in GC-IMS. For this purpose, two different GC-IMS data examples (urine and olive oil) are used to show the performance of the proposed method. The outputs of the algorithm are GC-IMS chromatogram with detected peaks, persistence plot showing the importance (intensity) of the detected peaks and a table with retention times (RT), drift times (DT), and persistence scores of detected peaks. The RT and DT can be used for identification of the peaks and persistence scores for quantitation. Additionally, watershed segmentation is applied to the GC-IMS images to index individual peaks and segment overlapping compounds allowing for a more accurate identification and quantification of individual peaks., Significance: Inspection of the results for GC-IMS datasets showed the accurate and reliable performance of the proposed strategy based on persistent homology for automatic 2D GC-IMS peak detection for qualitative and quantitative analysis. In addition, this approach can be easily extended to other types of hyphenated chromatographic and/or spectroscopic data., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

A head space-solid phase microextraction-gas chromatography-mass spectrometery (HS-SPME-GC-MS) method for the simultaneous analysis of pentene dimers from lipoxygenase (LOX) pathway, monoterpenes, and sesquiterpenes in extra virgin olive oil (EVOO) was proposed. A Doehlert design was performed; the conditions of the HS-SPME preconcentration step (extraction temperature, extraction time, sample amount, and desorption time) were optimized by response surface methodology, allowing defining the method operable design region. A quantitative method was set up using the multiple internal standard normalization approach: four internal standards were used, and the most suitable one was selected for area normalization of each external standard. The quantitative method was successfully validated and applied to a series of monocultivar EVOOs. This is the first paper in which a quantitative method using commercial standards has been proposed for the analysis of an important class of molecules of EVOO such as pentene dimers. The optimized method is suitable for routine analysis aimed at characterizing high quality EVOOs.

Leaves incorporation during the extraction of olive oils can enhance their chemical-sensory quality. Thus, leaves from cvs. Arbequina or Santulhana were added (1%, w/w) during the extraction of Arbequina oils using an Abencor system, being discussed the impacts on the phenolics and volatiles formation enzymatic pathways. Leaves addition contributed to a significant decrease (P-value < 0.05) of the contents of secoiridoids (-11%), C6-aldehydes (-16%), and ester compounds (-22%). This could be tentatively related to a reduction of the enzymatic activity of secoiridoids biosynthesis and lipoxygenase pathways, promoted by the leaves' addition. Moreover, in the presence of leaves, the oils' total contents of phenolics and volatiles were significantly reduced (-7 and -17%, respectively). Contrary, the incorporation of leaves significantly increased (P-value < 0.05) the contents of C6-alcohols (+37%) and the intensities of the green fruity (+25%) and apple (+30%) sensations., (Copyright © 2022 Elsevier Ltd. All rights reserved.)

Extra virgin olive oil (EVOO) is the best vegetable oil worldwide but, at the same time, is one of the product victims of fraud in the agri-food sector, and the differences about quality within the extra-virgin olive oil category are often missed. Several scientific techniques were applied in order to guarantee the authenticity and quality of this EVOO. In the present study, the volatile compounds (VOCs) by gas chromatography-mass spectrometry with solid-phase micro-extraction detection (GC-MS SPME), organoleptic analysis by the official Slow Food panel and the detection by a Small Sensor System (S3) were applied. Ten EVOOs from Umbria, a central Italian region, were selected from the 2021 Slow Food Italian extra virgin olive oil official guide, which includes hundreds of high-quality olive oils. The results demonstrated the possibility to discriminate the ten EVOOs, even if they belong to the same Italian region, by all three techniques. The result of GC-MS SPME detection was comparable at the discrimination level to the organoleptic test with few exceptions, while the S3 was able to better separate some EVOOs, which were not discriminated perfectly by the other two methods. The correlation analysis performed among and between the three methodologies allowed us to identify 388 strong associations with a p value less than 0.05. This study has highlighted how much the mix of VOCs was different even among few and localized EVOOs. The correlation with the sensor detection, which is faster and chipper compared to the other two techniques, elucidated the similarities and discrepancies between the applied methods., Competing Interests: The authors declare no conflict of interest.

Green glass (GG), ultraviolet grade absorbing glass (UVAGG), and multilayer (plastic-coated paperboard aluminium foil) (MLP) packagings were used for storing two commercially extra virgin olive oils (EVOOs) with different phenolic and volatile compound contents to evaluate their effect on oil quality evolution over 10 months of light exposure. Quality parameters such as free acidity, peroxide value, spectrophotometric indices, antioxidant and volatile compositions as well as sensory characteristics were evaluated; packaging material type and initial antioxidant composition significantly influenced EVOOs' resistance to oxidation, and consequently their quality. Compared with GG or UVAGG, MLP provided superior protection against oxidation; oils stored in MLP containers retained their characteristics within the regulatory limits and contained more antioxidants and fewer 'rancid' defect and related volatile compounds., (Copyright © 2021 Elsevier Ltd. All rights reserved.)

An olive pomace from the two-phase decanter stored in different conditions was used as a model to simulate the detrimental biological phenomena occurring during olive oil processing and storage. A group of EVOO and defective oils were also analyzed. The volatile fraction was studied with HS-SPME-GC-MS; 127 volatiles were identified (55 of which tentatively identified) and evaluated over time. Seven volatiles were tentatively identified for the first time in olive oil; the role of C6 alcohols in detrimental biological phenomena was highlighted. Suitable volatile markers for defects of microbiological origin were defined, particularly the fusty/muddy sediment. They were then applied to olive oils with different quality categories; one of the markers was able to discriminate among EVOOs and all the defective samples, including the borderline ones. The marker was constituted by the sum of concentrations of 10 esters, 4 alcohols, 1 ketone, and 1 α-hydroxy-ketone but no carboxylic acids.

Volatile organic compounds strongly contribute to both the positive and negative sensory attributes of virgin olive oil, and more and more studies have been published in recent years focusing on several aspects regarding these molecules. This Review is aimed at giving an overview on the state of the art about the virgin olive oil volatile compounds. Particular emphasis was given to the composition of the volatile fraction, the analytical issues and approaches for analysis, the sensory characteristics and interaction with phenolic compounds, and the approaches for supporting the Panel Test in virgin olive oil classification and in authentication of the botanical and geographic origin based on volatile compounds. A pair of detailed tables with a total of approximately 700 volatiles identified or tentatively identified to date and tables dealing with analytical procedures, sensory characteristics of volatiles, and specific chemometric approaches for quality assessment are also provided.

Three factors for the extraction of extra virgin olive oil (EVOO) were evaluated: diameter of the grid holes of the hammer-crusher, malaxation temperature, and malaxation time. A Box-Behnken design was used to obtain a total of 289 olive oil samples. Twelve responses were analyzed and 204 mathematical models were obtained. Olives from super-intensive rainfed or irrigated crops of the Arbequina, Koroneiki, and Arbosana cultivars at different stages of ripening were used. Malaxation temperature was found to be the factor with the most influence on the total content of lipoxygenase pathway volatile compounds; as the temperature increased, the content of volatile compounds decreased. On the contrary, pigments increased when the malaxation temperature was increased. EVOO from irrigated crops and from the Arbequina cultivar had the highest content of volatile compounds. Olive samples with a lower ripening degree, from the Koroneiki cultivar and from rainfed crops, had the highest content of pigments.

Background: Innovative technologies are experimentally applied to the virgin olive oil extraction process in order to make it continuous and more efficient. Most of the efforts aim at overcoming the limitations of the traditional malaxation step, which, however, is essential for the development of virgin olive oil sensory notes., Results: Compared to the traditional process, innovative technologies based on the heat exchanger led generally to a decrement in volatile lipoxygenase (LOX) alcohols linked to alcohol dehydrogenase activity and, conversely, to a slightly increase in volatile LOX esters. Aldehydes from the same pathway were not significantly affected. However, an industrial combined plant constructed from a heat exchanger, low-frequency ultrasound device and microwave apparatus determined the highest 'fruity' intensity perceived by panellists, in accordance with the highest value of total volatiles, with values significantly higher than heat exchanger alone, which, instead, had the lowest levels of hexanal and LOX alcohols. The pungent taste showed the same trend observed for 'fruity' intensity, whereas bitter taste did not show significant differences among trials., Conclusion: The introduction of ultrasound, coupled with heat exchanger and microwave, seemed not to modify the behaviour of enzymes of the LOX pathway, and the obtained virgin olive oils showed volatiles and organoleptic characteristics not significantly different from those obtained by the traditional olive oil extraction process. These findings provided the first insights into the effect of the combination of innovative technologies in the olive oil extraction process on virgin olive oil volatiles and sensory characteristics. © 2019 Society of Chemical Industry., (© 2019 Society of Chemical Industry.)

Aroma profiles, key aroma compound quantification, and cluster analysis of 15 brands of extra-virgin olive oils (EVOOs) from three countries (Spain, Italy, and Greece) were investigated in the current study. Aroma compounds were isolated from the oil by using solvent-assisted flavor evaporation (SAFE) and solid-phase micro-extraction (SPME) and analyzed by gas chromatography-olfactometry mass spectrometry (GC-MS/O). A total of 89 compounds were screened by SPME/SAFE-GC-MS/O with chromatographic columns in 15 brands of samples. Eighty and 54 compounds were respectively identified by SPME- and SAFE-GC-MS/O. Of those, 44 compounds were detected by both methods. Undecanol, (Z)-4-decenal, (E)-2-dodecenal, and 2-nonanone extracted by SAFE were not found in EVOOs before. Eight classes of aroma compounds were identified, including 17 alcohols, 22 aldehydes, 9 ketones, 4 acids, 14 esters, 5 aromatics, 12 alkene, and 6 others. Eleven compounds were identified as the key aroma compounds in alternative brands of EVOOs by SAFE-aroma extract dilution analysis (AEDA). Hexanal, (E)-2-hexenal, (E)-3-hexenol, acetic acid, and (E)-2-heptenal were the common key aroma compounds by AEDA and odor activity values (OAVs). From the cluster analysis of the heatmap, the aroma compounds of all the Spain EVOOs were similar, and there were some differences from the samples of Italy and Greece. It suggested that both the amount and concentration of aroma compounds determine the similarity of aroma in EVOOs.

Competition and interaction phenomena among volatiles during their adsorption process by solid phase microextraction (SPME) fibers in static headspace sampling procedure (SHS) cast doubt on its ability to quantify virgin olive oil volatiles. SPME fibers being excellent traps, their use was analyzed with a new device allowing the concentration of volatiles in a dynamic headspace sampling procedure (DHS). A central composite experimental design optimized the main variables of the device (4 g sample weight, 40 °C temperature, 150 mL/min flow rate, 50 min adsorption time), while values of the analytical quality control parameters of the method (repeatability, limits of detection and quantification, working range, sensitivity, and resolution) were compared with those ones from static headspace. DHS shows better precision results for aldehydes and alcohols than SHS and allowed analyzing higher concentrations with no problem of saturation. In 19 of 28 compounds analyzed in 50 samples the chromatographic areas were higher when running DHS. The concentration values of volatile compounds in these samples after applying SHS and DHS are discussed together with the ability of the new method for distinguishing virgin olive oil by their categories (extra virgin, virgin, and lampante) by the volatiles quantified in commercial oils.

The virgin olive oils (VOOs) under examination were from the main Tunisian cultivar 'Chemlali'. Olive fruits used for oil production were stored in plastic containers for four weeks at ambient temperature. Hydrophilic bioactive compounds and volatile profiles of the corresponding oils were analyzed. Chemometric analysis showed that VOO obtained from fruits stored during one week is similar to that of freshly harvested fruits. They preserved their bioactive and volatile molecular markers of freshness with the predominance of the secoiridoid aldehydic form of oleuropeine aglycon, and the C 6 lipoxygenase products. However, VOO obtained from fruits stored for a long time, showed degradation of the derivatives of oleuropeine and ligstroside aglycons, a decrease in the lignan, and flavonoid groups, whereas phenolic acids showed a remarkable increase. The volatile profile was characterized by a decrease in the LOX products, and biosynthesis of the volatile molecular markers of oxidation C 7 -C 10 aldehydes (nonanal, decanal, (Z) and (E)-2-heptenal, (E)-2-octenal, and (E,E)-2,4-heptadienal), and hydrocarbons (n-dodecane, and n-tetradecane). Mono and sesquiterpenes showed also an increase over storage time. Consequently, and in order to avoid deterioration of VOO composition, chemometric analysis showed that the olive fruits should be processed as soon as possible after being harvested, with a maximum storage time of one week., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

In this study, atmospheric pressure chemical ionisation-mass spectrometry (APCI-MS) was successfully applied to understand the effect of phenolic compounds on the release of olive oil aroma compounds. Eight aroma compounds were monitored under in-vivo and in-vitro dynamic conditions in olive oil with and without the addition of virgin olive oil (VOO) biophenols. Three model olive oils (MOOs) were set up with identical volatile compounds concentrations using a refined olive oil (ROO). Phenolics were extracted from VOOs and were added to two MOOs in order to obtain two different concentrations of phenolic compounds (P+ = 354 mg kg -1 ; P++ = 593 mg kg -1 ). Another MOO was without VOO biophenols (P-). Phenolic compounds impacted both the intensity and time of aroma release. In the in-vivo study, 1-penten-3-one, trans-2-hexenal and esters had lower release in the presence of higher levels of biophenols after swallowing. In contrast, linalool and 1-hexanol had a greater release. The more hydrophobic compounds had a longer persistence in the breath than the hydrophilic compounds. VOO phenolics-proline-rich proteins complexes could explain the binding of aroma compounds and consequently their decrease during analysis and during organoleptic assessment of olive oil., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

The approach of this research was to describe the biochemical transformations of minor components of virgin olive oil with high impact on its sensory quality, specifically "volatile compounds" during its extraction process. For this purpose `Picual´, `Arbequina´ and `Hojiblanca´ cultivars were processed at three different harvesting times. Their volatile profiles and levels of enzymatic activity of "hydroperoxide lyase", responsible for the biosynthesis of C6 aldehydes related to "green and fruity notes", were monitored and identified in mesocarp, paste before kneading and paste after kneading based on the catalytic action of crude enzyme extracts. Both of them, volatiles and HPL, were analyzed by incubating with their corresponding substrates and reaction products formed were analyzed by Solid Phase Microextraction-Gas Chromatography and Mass Spectrometry. The results obtained in the present research can be useful in order to develop new markers biochemical whereby improved aroma quality in olive breeding programs or in the design of new protocol of VOO extraction., (Published by Elsevier Ltd.)

A quantitative method, based on SPME GC-MS, for the quantification of volatile compounds derived from lipoxygenase pathway, considered the most important for the aroma of high-quality olive oil, was developed. The method was used to study the variation within the extra virgin olive oils from 67 cultivars of the Tuscan olive germplasm conserved at "Santa Paolina" experimental farm (Follonica, Italy). A great variability was observed among the 67 cultivars both for the total amount of volatile compounds and for the different ratios between the groups of volatile compounds from common precursors. The aim was to obtain basic information on the characteristics and the quality of the oils obtainable from nonwidely cultivated olive varieties. These data can support the reintroduction in the production chain of old autochthonous varieties and for exploitation in breeding programs as a source of positive characters to transmit to the progeny., (© 2018 John Wiley & Sons, Ltd.)

Background: The organoleptic quality of virgin olive oil depends on positive and negative sensory attributes. These attributes are related to volatile organic compounds and phenolic compounds that represent the aroma and taste (flavour) of the virgin olive oil. The flavour is the characteristic that can be measured by a taster panel. However, as for any analytical measuring device, the tasters, individually, and the panel, as a whole, should be harmonized and validated and proper olive oil standards are needed., Results: In the present study, multivariate approaches are put into practice in addition to the rules to build a multivariate control chart from chromatographic volatile fingerprinting and chemometrics. Fingerprinting techniques provide analytical information without identify and quantify the analytes. This methodology is used to monitor the stability of sensory reference materials., Conclusion: The similarity indices have been calculated to build multivariate control chart with two olive oils certified reference materials that have been used as examples to monitor their stabilities. This methodology with chromatographic data could be applied in parallel with the 'panel test' sensory method to reduce the work of sensory analysis. © 2018 Society of Chemical Industry., (© 2018 Society of Chemical Industry.)

This study focused on the volatile changes in cv. Verdeal Transmontana throughout the entire olive oil processing chain, from the drupe to olive oil storage up to 12 months, while correlating it with quality parameters and sensory quality. During crushing and malaxation, the volatiles formed were mainly "green-leaf volatiles" (GLVs), namely (E)-2-hexenal, hexanal, and 1-hexanol. Centrifugation and clarification steps increased the total volatile amounts to 130 mg kg -1 . However, clarification also increased nonanal and (E)-2-decenal contents, two markers of oxidation, with a noticeable loss of phenolic compounds and oxidative stability. During storage, the total volatile amounts reduced drastically (94% at 12 months after extraction), together with the positive sensory attributes fruity, green, bitter, and pungent. Despite being classified as extra-virgin after one year of storage, peroxides and conjugated dienes were significantly higher while there was a reduction in antioxidant capacity as well as in phenolic compounds (less 50%) and oxidative stability (57%). The present work allowed concluding that the extraction process modulates the volatile composition of olive oil, with a concentration of volatiles at the clarification step. During storage, volatiles are lost, mainly eight months after extraction, leading to the loss of important sensory attributes., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

De-stoning technology has been introduced in the olive oil sector more than twenty years ago. It has not gained momentum because, sometimes, innovative ideas are not accepted since they are suggested at the wrong time or under the wrong circumstances. Virgin olive oil (VOO) is one of the most popular functional foods, mainly due to its antioxidant properties. These features, as well as other nutritional characteristics are generally enhanced by the de-stoning process. However, despite the improvement of the nutritional value, in the past the de-stoned oil didn't achieve marketing success mainly in relation to technological limitations (i.e. low oil yield). Only in recent years healthy properties became an element able to influence consumers' behavior, overcoming the limit of low oil yields and attracting the attention of olive oil producers. An analysis of the advantages, in terms of product quality and process sustainability, is given in this review. Here, for the first time, the fragmented results reported in literature are critically analyzed underlining the contradictions reported by different authors showing the main reasons for the unlucky fate of this technology in the industrial sector. In the final section the challenges, that future research must focus on, are presented, including emerging technologies in VOO processing. Literature data, for the first time discussed here exhaustively, show that de-stoning technology is a mechanical strategy useful to increase the nutritional and the sensory quality of the product. Moreover, it reduces the depletion of natural resources obtaining a selective crushing of the drupe by removing the stones from the olive paste so increasing the sustainability and efficiency of VOO extraction plants., (Copyright © 2018 Elsevier Ltd. All rights reserved.)

Crushing is a key step during olive oil extraction. Among commercial crushers, the hammer mill is the most widely used due to its robustness and high throughput. In the present work, the impact of hammer mill rotor speed on extraction yield and overall quality of super-high-density Arbosana olive oils were assessed in an industrial facility. Our results show that increasing the rotor speed from 2400rpm to 3600rpm led to a rise in oil yield of 1.2%, while conserving quality parameters. Sensory analysis showed more pungency with increased rotation speed, while others attributes were unaffected. Volatile compounds showed little variation with the differences in crusher speed; however, total phenols content, two relevant secoiridoids, and triterpenoids levels increased with rotor speed. Hammer mill rotor speed is a processing variable that can be tuned to increase the extraction efficiency and modulate the chemical composition of extra virgin olive oil., (Copyright © 2017 Elsevier Ltd. All rights reserved.)

Freeze injuries in olives are responsible for the 'frostbitten olives' sensory defect that is sometimes detected in virgin olive oil. This defect is becoming one of the most common negative attributes today because climate change has modified weather patterns. The temperature changes can take place abruptly, with rapid freeze-thaw cycles, or gradually. These changes produce significant alterations in the quality of the oils. This study analyzed the volatile composition of virgin olive oils characterized with 'frostbitten olives' defect. The volatile information allowed grouping these oils into two types characterized with two different profiles. One of them is characterized by 'soapy' and 'strawberry-like' perceptions and the presence of two volatile compounds (ethyl 2-methyl butanoate and ethyl propanoate). The second profile is characterized by 'wood' and 'humidity' descriptors and a high concentration of two volatiles (pentanal and octanal). These results on volatiles explain the existence of two sensory profiles associated with the 'frostbitten olives' defect.

The commercial value of virgin olive oils (VOOs) strongly depends on their classification, also based on the aroma of the oils, usually evaluated by a panel test. Nowadays, a reliable analytical method is still needed to evaluate the volatile organic compounds (VOCs) and support the standard panel test method. To date, the use of HS-SPME sampling coupled to GC-MS is generally accepted for the analysis of VOCs in VOOs. However, VOO is a challenging matrix due to the simultaneous presence of: i) compounds at ppm and ppb concentrations; ii) molecules belonging to different chemical classes and iii) analytes with a wide range of molecular mass. Therefore, HS-SPME-GC-MS quantitation based upon the use of external standard method or of only a single internal standard (ISTD) for data normalization in an internal standard method, may be troublesome. In this work a multiple internal standard normalization is proposed to overcome these problems and improving quantitation of VOO-VOCs. As many as 11 ISTDs were used for quantitation of 71 VOCs. For each of them the most suitable ISTD was selected and a good linearity in a wide range of calibration was obtained. Except for E-2-hexenal, without ISTD or with an unsuitable ISTD, the linear range of calibration was narrower with respect to that obtained by a suitable ISTD, confirming the usefulness of multiple internal standard normalization for the correct quantitation of VOCs profile in VOOs. The method was validated for 71 VOCs, and then applied to a series of lampante virgin olive oils and extra virgin olive oils. In light of our results, we propose the application of this analytical approach for routine quantitative analyses and to support sensorial analysis for the evaluation of positive and negative VOOs attributes., (Copyright © 2017 Elsevier B.V. All rights reserved.)

The novel atmospheric pressure chemical ionization (APCI) source has been used in combination with gas chromatography (GC) coupled to hybrid quadrupole time-of-flight (QTOF) mass spectrometry (MS) for determination of volatile components of olive oil, enhancing its potential for classification of olive oil samples according to their quality using a metabolomics-based approach. The full-spectrum acquisition has allowed the detection of volatile organic compounds (VOCs) in olive oil samples, including Extra Virgin, Virgin and Lampante qualities. A dynamic headspace extraction with cartridge solvent elution was applied. The metabolomics strategy consisted of three different steps: a full mass spectral alignment of GC-MS data using MzMine 2.0, a multivariate analysis using Ez-Info and the creation of the statistical model with combinations of responses for molecular fragments. The model was finally validated using blind samples, obtaining an accuracy in oil classification of 70%, taking the official established method, "PANEL TEST", as reference., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

It was previously demonstrated that Fourier transform near infrared (FT-NIR) spectroscopy and partial least squares (PLS1) were successfully used to assess whether an olive oil was extra virgin, and if adulterated, with which type of vegetable oil and by how much using previously developed PLS1 calibration models. This last prediction required an initial set of four PLS1 calibration models that were based on gravimetrically prepared mixtures of a specific variety of extra virgin olive oil (EVOO) spiked with adulterants. The current study was undertaken after obtaining a range of EVOO varieties grown in different countries. It was found that all the different types of EVOO varieties investigated belonged to four distinct groups, and each required the development of additional sets of specific PLS1 calibration models to ensure that they can be used to predict low concentrations of vegetable oils high in linoleic, oleic, or palmitic acid, and/or refined olive oil. These four distinct sets of PLS1 calibration models were required to cover the range of EVOO varieties with a linoleic acid content from 1.3 to 15.5 % of total fatty acids. An FT-NIR library was established with 66 EVOO products obtained from California and Europe. The quality and/or purity of EVOO were assessed by determining the FT-NIR Index, a measure of the volatile content of EVOO. The use of these PLS1 calibration models made it possible to predict the authenticity of EVOO and the identity and quantity of potential adulterant oils in minutes.

The distinctive aroma of virgin olive oil is mainly attributed to its volatile profile including components responsible for positive attributes and others for sensory defects resulting from chemical oxidation and exogenous enzymes. For this reason, the evolution of volatile compounds from Chétoui and Arbequina virgin olive oils during olive ripening and storage (at 4 and 25 °C during 4 weeks) was investigated. The profile of volatile phenols during olive storage was also studied. Quantitative differences in the volatile compounds during olive storage at 4 and 25 °C according to olive cultivar was determined. Concerning the volatile phenols, the Arbequina olives were the most affected by high storage temperature, as the formation of these compounds, especially 4-ethyl and 4-vinyl derivatives of phenol and guaiacol were more noticeable in Arbequina oils extracted from stored fruits at 25 °C., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

Olive oil flavouring with aromatic plants and spices is a traditional practice in Mediterranean gastronomy. The aim of this work was to compare the influence of two different flavouring techniques (infusion of spices into the oil vs. combined malaxation of olives paste and spices) on chemical and sensory quality of flavoured olive oil. In particular, oxidative and hydrolytic degradation (by routine and non-conventional analyses), phenolic profiles (by HPLC), volatile compounds (by SPME-GC/MS), antioxidant activity, and sensory properties (by a trained panel and by consumers) of the oils were evaluated. The obtained results evidenced that the malaxation method was more effective in extracting the phenolic compounds, with a significantly lower level of hydrolysis of secoiridoids. As a consequence, antioxidant activity was significantly lower in the oils obtained by infusion, which were characterized by a higher extent of the oxidative degradation. The volatile compounds were not significantly influenced by changing the flavouring method, apart for sulfur compounds that were more abundant in the oils obtained by the combined malaxation method. From a sensory point of view, more intense bitter and pungent tastes were perceived when the infusion method was adopted., (Copyright © 2016 Elsevier Ltd. All rights reserved.)

The influence of filtration through a hydrophilic cotton layer on volatile compounds, sensory characteristics and colour of two monovarietal oils was investigated in this study. Volatiles were evaluated using headspace solid-phase microextraction-gas chromatography. After the filtration of Buža oils only a slight increase in total alcohols was noticed. In filtered Črna oils a significant decrease of total alcohols and slight changes in total aldehydes, total ketones and total C5 volatile compounds concentration were detected. No significant influence on the sensory scores of oils, but some slight changes in sensorial profiles were noted (slightly higher intensities of sensory characteristics apple and grass, and higher values of the lightness L(∗) in filtered samples). The results point to unequal filtration impact on different monovarietal oils and could be useful in developing targeted technologies for specific monovarietal oils quality improvement., (Copyright © 2011 Elsevier Ltd. All rights reserved.)

In order to investigate the relationship between the occurrence of the "grubby" sensory defect caused by olive fruit fly (Bactrocera oleae (Rossi)) infestation and the resulting volatile composition, virgin olive oils were extracted from olives of the Leccino cultivar with 0%, 50%, and 100% olive fly infestations and subjected to analysis of the basic chemical quality parameters, fatty acids and volatiles, and sensory analysis by the Panel test. A 100% olive fly infestation reduced the basic chemical quality of the oil, while the fatty acid composition was not affected in any case. The overall sensory quality score and intensity of the positive sensory attributes decreased, while the intensity of the "grubby" defect increased proportionally to the degree of infestation. The occurrence and intensity of this defect were clearly causally related to the concentrations of 3-methylbutanal, 2-methylbutanal, β-ocimene, ethyl 2-methylbutyrate, dimethyl sulfoxide, 4-methyl-5H-furan-2-one, α-farnesene, 6-methyl-5-hepten-2-one, 1-octanol, E-2-nonen-1-ol, benzeneacetaldehyde, heptanal, and octanal, implying that the perception of "grubby" comes from their joint contribution to the overall olive oil flavour. In addition to contributing to the understanding of the chemical origin of "grubby", the results obtained could potentially be used to develop strategies to support sensory analysis in the classification of olive oil quality and the confirmation of the presence of this sensory defect in oil samples. [ABSTRACT FROM AUTHOR]

The investigation of volatile compounds in the headspace of liquid samples can often be used for detailed and non-destructive characterisation of the sample. This has great potential for process control or the characterisation of food samples, such as olive oil. We investigated, for the first time, the plume of substances released from olive oil droplets by laser desorption in a feasibility study and applied ion mobility spectrometry coupled to rapid GC pre-separation to enhance selectivity. Our investigation demonstrated that significantly more substances can be detected and quantified via laser desorption than in the usual headspace, enabling a rapid (5–10 min), sensitive (low ng/g range) and comprehensive analysis of the sample, with the potential for quality control and fraud identification. Therefore, laser desorption provides a useful sampling tool for characterising liquids in many applications, requiring only a few µL of sample. [ABSTRACT FROM AUTHOR]

The capability of determining the phenolic and volatile profiles of olive oils is of major relevance since these compounds are known to greatly influence the gustatory and olfactory positive attributes of olive oils. An electronic tongue with multiple linear regression models was used to evaluate both profiles based on olive oils potentiometric data generated during a single assay. The proposed electronic tongue-chemometric procedure enabled the quantification of flavonoids, phenolic acids and phenol alcohols of Arbequina extra-virgin olive oils with a similar accuracy of UPLC-MS (0.93 ± 0.03 ≤  R 2  ≤ 0.98 ± 0.08 for the repeated K-fold cross-validation procedure). Also, it was verified that the potentiometric device should not be applied to evaluate volatile compounds in solution (0.80 ± 0.14 ≤  R 2  ≤ 0.94 ± 0.05 for the repeated K-fold cross-validation procedure), showing a lower accuracy than HS-SPME-GS-MS. The overall satisfactory results showed that electronic tongue could be used as a practical sensing instrument to generate a chemical profile of the compounds known to influence the positive sensory attributes of olive oils. [ABSTRACT FROM AUTHOR]

In this work the emission of volatile organic compounds (VOCs) upon the heating process of an extra virgin olive oil (EVOO) and a high oleic sunflower oil (SFO) was evaluated in real time by spectrometry. Two tests were carried out, in the first VOCs emitted from both kinds of oil were measured at room temperatures (not heated, NH) and at 180°C; in the second test, VOCs emission for selected masses were monitored under increasing temperatures over time: at room temperature not heated oils (NH), 60, 90, 120, 150, and 180°C, respectively. The spectra were acquired using a Proton Transfer Reaction Time of Flight Mass Spectrometer (PTR-ToF-MS). The total VOCs emission increased at 180°C, determined both by the rise of the amount of compounds present in the NH samples and by the formation of new masses generated by oxidative chemical reaction from triglycerides and fatty acids. From the set of results it is evident that a good control of the temperatures can be useful in reducing the quantities of masses potentially harmful to health in human food. [ABSTRACT FROM AUTHOR]

This work aims at presenting the state-of-the-art about the influence of the activity of olive endogenous enzymes, as well as of the application of adjuvants in olive oil technology, discussing their influence on the composition of virgin olive oil, especially in phenols and volatile compounds. [ABSTRACT FROM AUTHOR]

The aim of the study was to assess the influence of talc on the extra virgin olive oil volatile profile during production and storage. The obtained results showed that talc used at 1% level did not cause significant differences, whereas at 2% level showed only slight differences were revealed compared to control. During storage a significant increase of the volatiles deriving from the oxidative process was observed and a concomitant significant decrease of the C6-LOX aldehydes. The evolution of the volatile compounds of extra virgin olive oils during storage was not significantly influenced by talc addition, with the exception of the sum of C6-LOX aldehydes, which showed a significant higher decrease. [ABSTRACT FROM AUTHOR]

Chemometric discrimination of extra virgin olive oils (EVOO) from whole and stoned olive pastes was carried out by using Fourier transform infrared (FTIR) data and partial least squares-discriminant analysis (PLS1-DA) approach. Four Italian commercial EVOO brands, all in both whole and stoned version, were considered in this study. The adopted chemometric methodologies were able to describe the different chemical features in phenolic and volatile compounds contained in the two types of oil by using unspecific IR spectral information. Principal component analysis (PCA) was employed in cluster analysis to capture data patterns and to highlight differences between technological processes and EVOO brands. The PLS1-DA algorithm was used as supervised discriminant analysis to identify the different oil extraction procedures. Discriminant analysis was extended to the evaluation of possible adulteration by addition of aliquots of oil from whole paste to the most valuable oil from stoned olives. The statistical parameters from external validation of all the PLS models were very satisfactory, with low root mean square error of prediction (RMSEP) and relative error (RE%). [ABSTRACT FROM AUTHOR]

Continuous application of high power ultrasound (HPU) on olive paste previous to malaxation at laboratory scale for virgin olive oil (VOO) extraction and its effect on process yield and the VOO quality have been studied. For the VOO samples, we determined the quality indices (free acidity value, peroxide value, K232, K270), bitterness, volatile composition, phenolic content (total and biophenols), tocopherol content, and pigments. The application of ultrasound induced a quick heating of the paste from 20 to 28°C. The sonication treatment improved the industrial oil yield by 1% and the oil extractability by 5.74%. Moreover the HPU treatment did not cause changes in the quality indices, fatty acid composition and volatile aromatic compounds of the VOO. Furthermore the fat autoxidation process was not accelerated by this treatment. Meanwhile oil obtained from olive pastes treated with HPU showed higher content of tocopherol, chlorophylls and carotenoids whereas a reduction in phenolic content and bitterness index was observed. Practical applications: The high power ultrasound (HPU) treatment of olive paste, before malaxation during the virgin olive oil (VOO) elaboration process, can improve the oil extraction yield without alteration of its quality parameters. The olive paste instantaneous heating observed with the HPU can allow the reduction of the malaxation step duration. The results obtained nowadays at laboratory scale are promising for the possibility of the continuous HPU treatment introduction in the olive oil elaboration process as aid or alternative to the malaxation. For this purpose further experiment at pilot and industrial scale are needed. Continuous application of high power ultrasound before malaxation and its effect on the oil extractability and virgin olive oil characteristics. [ABSTRACT FROM AUTHOR]

The new health claim on 'olive oil polyphenols' recently approved by the European Commission has produced a dramatic increase in the interest in these antioxidant compounds. Although this interest has been focused mostly on extra virgin olive oils (EVOOs), virgin olive oils (VOOs) qualified as having non-oxidative sensory defects, mostly caused by fermentation and the action of fungi on olives, may still have a considerable amount of phenols, even though their sensory quality is not flawless. This study is focused on the phenol composition of all the VOO categories: EVOOs with their ample variability in phenolic composition, VOOs with slight defects, lampante virgin olive oils (LVOO), and reference materials of defective VOOs. The average content of phenols in the analyzed EVOOs (410 ± 16 mg/kg) is higher than the recommended consumption by the health claim (250 mg/kg). VOOs qualified with non-oxidative defects contain high concentrations of phenols (234 ± 27 mg/kg), but only samples characterized by the wet-wood sensory defect show concentrations of phenols close to 250 mg/kg. Practical application: This study has demonstrated that VOOs with slight sensory defects still have a high concentration of phenols, providing antioxidant properties regarding health benefits and stability. The health claim should be not only applied to the extra virgin olive oil category, but also to some virgin olive oils with sensory defects. Profiles of phenols according to their main sensory defect. Picual (A), Hojiblanca (B), rancid (C), winey-vinegary (D), fusty (E), and musty (F). [ABSTRACT FROM AUTHOR]

BACKGROUND: The volatile fraction of virgin olive oil is characterised by low molecular weight compounds that vaporise at room temperature. In order to obtain an aroma profile similar to natural olfactory perception, the composition of the volatile compounds was determined by applying dynamic headspace gas chromatography, performed at room temperature, with a cryogenic trap directly connected to a gas chromatograph--mass spectrometer system. Samples were also evaluated according to European Union and International Olive Council official methods for sensory evaluation. In this paper, the composition of the volatile fraction of 25 extra virgin olive oils from different regions of Italy was analysed and some preliminary considerations on relationships between chemical composition of volatile fraction and sensory characteristics are reported. RESULTS: Forty-two compounds were identified by means of the particular analytical technique used. All the analysed samples, classified as extra virgin by the panel test, never present peaks whose magnitude is important enough in defected oils. The study was focused on the evaluation of volatile compounds responsible for the positive impact on olive odour properties ('green--fruity' and 'sweet') and olfactory perception. CONCLUSION: Chemometric evaluation of data, obtained through headspace analysis and the panel test evaluation, showed a correlation between chemical compounds and sensory properties. On the basis of the results, the positive attributes of virgin olive oil are divided into two separated groups: sweet types or green types. Sixteen volatile compounds with known positive impact on odour properties were extracted and identified. In particular, eight compounds seem correlated with sweet properties whereas the green sensation appears to be correlated with eight other different substances. The content of the compounds at six carbon atoms proves to be very important in defining positive attributes of extra virgin olive oils and sensory evaluation. [ABSTRACT FROM AUTHOR]

Volatile compounds are responsible for most of the sensory qualities of virgin olive oil and they are synthesized when enzymes and substrates come together as olive fruit is crushed during the industrial process to obtain the oil. Here we have studied the variability among the major volatile compounds in virgin olive oil prepared from the progeny of a cross of Picual and Arbequina olive cultivars ( Olea europaea L.). The volatile compounds were isolated by SPME, and analyzed by HRGC–MS and HRGC–FID. Most of the volatile compounds found in the progeny's oil are produced by the enzymes in the so-called lipoxygenase pathway, and they may be clustered into different groups according to their chain length and polyunsaturated fatty acid origin (linoleic and linolenic acids). In addition, a group of compounds derived from amino acid metabolism and two terpenes also contributed significantly to the volatile fraction, some of which had significant odor values in most of the genotypes evaluated. The volatile compound content of the progeny was very varied, widely transgressing the progenitor levels, suggesting that in breeding programs it might be more effective to consider a larger number of individuals within the same cross than using different crosses with fewer individuals. Multivariate analysis allowed genotypes with particularly interesting volatile compositions to be identified and their flavor quality deduced. [ABSTRACT FROM AUTHOR]

The characterisation of different olive oil categories (extra virgin, virgin and lampante) using Ion Mobility Spectrometry (IMS) was improved by replacing the multicapillary column (MCC) with a capillary column (CC). The data obtained with MCC–IMS and CC–IMS were evaluated, studying both the global and the specific information obtained after the analysis of the volatile fraction of olive oils. A better differentiation of the oil categories was obtained employing CC vs MCC, since the classification percentage obtained with the CC–IMS was 92% as opposed to 87% obtained with MCC–IMS; although in productivity analytical terms, MCC offer a faster analysis than GC. The specific information obtained was also used to build a database, with a view to facilitating the characterization of specific attributes of olive oils. A total of 26 volatile metabolites (aldehydes, ketones, alcohols and esters) were identified. Finally, as revealed by an ANOVA test, some volatiles differed markedly in content among the different categories of oil. The data obtained confirms the potential of IMS as a reliable analytical screening technique, which can be used to assign the correct category to an olive oil sample. [ABSTRACT FROM AUTHOR]

Second centrifugation of olive paste is often carried out to recover the residual oil of the olive paste, leading to a product that must be marketed as raw olive pomace oil. An experimental investigation was carried out to assess yield, chemical composition, and volatile compounds of oils obtained after the first and the second centrifugation of olive paste. Olives from Coratina cultivar were used in trials and were processed by adding 1 g/100 g and 2 g/100 g of technological coadjuvant micronized talc, as well as without talc addition, as control. The obtained results evidenced that the second centrifugation determined a significant decrease of residual oil in pomace. The addition of talc determined a significant increase of oil yield respect to control without talc, but only after the first centrifugation. A scarce increase of oil yield was observed after the second centrifugation, in presence of talc, that would render economically not viable the use of a second working line. Moreover, the oil obtained after the second centrifugation showed higher extent of oxidative and hydrolytic degradation than the oil from the first centrifugation. Some volatile compounds, derived from oxidative and fermentative phenomena, were observed in specific amounts in the oil of second centrifugation. [ABSTRACT FROM AUTHOR]

Highlights: [•] Analysis of olive oil flavored with truffles by DHS–GC–MS and electronic nose. [•] Blind analysis of oil flavored truffles taken from the Italian market. [•] Detected 63 volatile compounds, 32 from oil, 19 from truffle and 12 of other origin. [•] E-nose was able to discriminate the three species of truffle declared on the label. [•] Confirming the malpractice of the use of bismethyl(dithio)methane. [ABSTRACT FROM AUTHOR]