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Abstract This work implemented a non-invasive volatile organic compounds (VOCs) monitoring approach to study how food components are metabolised by the gut microbiota in-vitro. The fermentability of a model food matrix rich in dietary fibre (oat bran), and a pure prebiotic (inulin), added to a minimal gut medium was compared by looking at global changes in the volatilome. The substrates were incubated with a stabilised human faecal inoculum over a 24-h period, and VOCs were monitored without interfering with biological processes. The fermentation was performed in nitrogen-filled vials, with controlled temperature, and tracked by automated headspace-solid-phase microextraction coupled with gas chromatography–mass spectrometry. To understand the molecular patterns over time, we applied a multivariate longitudinal statistical framework: repeated measurements—ANOVA simultaneous component analysis. The methodology was able to discriminate the studied groups by looking at VOCs temporal profiles. The volatilome showed a time-dependency that was more distinct after 12 h. Short to medium-chain fatty acids showed increased peak intensities, mainly for oat bran and for inulin, but with different kinetics. At the same time, alcohols, aldehydes, and esters showed distinct trends with discriminatory power. The proposed approach can be applied to study the intertwined pathways of gut microbiota food components interaction in-vitro.

Terpenoids are a class of compounds found in hops which are responsible for the distinctive hop aromas in beer. Changes in terpenoid composition during fermentation as a result of yeast biotransformation influences beer aroma, but the pathways involved in these reactions are yet to be fully understood. In this study, eleven terpenoid standards (geraniol, nerol, citronellol, citral, α-terpineol, citronellyl acetate, caryophyllene, linalool, limonene, β-pinene and myrcene) were individually added to a model beer system fermented with commercially available Saccharomyces cerevisiae yeast (SafAle US-05). Volatile organic compounds (VOCs) were measured before and after fermentation with headspace solid-phase microextraction gas chromatography/mass spectrometry (SPME-GC/MS). Upon adding a single terpenoid standard to the model beer system, multiple terpenoid products were detected in the resulting beer at the end of fermentation. For example, when geraniol (10 ppm) was added, geraniol, citronellol, citronellyl acetate, citronellal, nerol, dihydrolinalool and dihydrocitronellol were detected at the end of fermentation. This research illustrates the importance of studying individual terpenoids as it provides valuable insights into the complex chemistry of beer. This information can aid in the optimisation of brewing to enhance the production of the flavours and aromas in beer desired by consumers.

Maize porridge, known as ''polenta'' in Italy, is a global staple food. This study aims to characterize the quality of four Italian flint maize landraces by investigating physical properties and macronutrients composition. By using SPME GC–MS and PTR-ToF-MS we analyzed the flours volatilome and changes in aroma profile post- cooking. Cooking induced the formation of 5 compounds and the loss of up to 25 compounds, primarily through evaporation. Post-cooking, the concentrations of some sulphur compounds (methanethiol, dimethyl sulfide and dimethyl trisulfide), lipid oxidation compounds (2-pentylfuran and hexanal) and Maillard reaction compounds including some aldehydes (nonanal, benzaldehyde, phenylacetaldheyde), pyridine and furans (furfural and furfuryl alcohol) increased. Differences in volatilome and macronutrients contents among landraces were also observed with Marano samples having on average a significantly higher concentration of proteins (13.67 %), while the Nostrano samples had the highest fat content (5.00 %). Fatty acid profile differences were mirrored in the volatilome. Spin flours had the highest level of linoleic acid, leading to elevated levels in cooked polenta due to linoleic acid oxidation. The differences in volatilome and macronutrients contents among the samples confirmed that local landraces are not only important for biodiversity and cultural heritage but also lead to unique aroma compounds profiles.

Bacterial fermentation is considered to be a cost-effective means of generating desired flavour compounds from plant-based substrates. However, the wide range of substrates present in plants makes it challenging to understand how individual components impact on flavour volatile organic compound (VOC) production. To simplify this, a defined medium can be used to better understand VOCs production with regard to individual compounds. In the current study, the VOCs produced by the lactic acid bacterium, Levilactobacillus brevis WLP672, growing in a defined medium containing different carbon sources (either glucose (DM), fructose (DMFr) or citrate (DMCi)) under a range of fermentation conditions (time: 0, 7, and 14 days; and temperature: 25 and 35 °C) were assessed using proton transfer reaction time-of-flight mass spectrometry (PTR-ToF-MS). Among the detected mass peaks (m/z), after 7 days of fermentation, the concentrations of m/z 45.033 (t.i. acetaldehyde), m/z 49.011 (t.i. methanethiol), and m/z 89.060 (t.i. ethyl acetate) were significantly (p < 0.05) higher in DM at 35 °C than all other treatments at either temperature. The knowledge obtained will help to produce desirable LAB fermentation flavour VOCs or VOC mixtures that could be used in developing plant-based analogues with acceptable sensory properties.

Lactic acid bacteria (LAB) fermentation is a viable approach for producing plant-based flavour compounds; however, little is understood about the impact of different LAB strains and medium compositions on the production of volatile organic compounds (VOCs). This study investigated the impact of the addition of individual amino acids (AAs) (L-leucine, L-isoleucine, L-phenylalanine, L-glutamic acid, L-aspartic acid, L-threonine, or L-methionine) to a defined medium (DM) on the generation of VOCs (after 0, 7, and 14 days) by one of three LAB strains (Levilactobacillus brevis WLP672 (LB672), Lactiplantibacillus plantarum LP100 (LP100), and Pediococcus pentosaceus PP100 (PP100)), using proton transfer reaction-time of flight-mass spectrometry (PTR-ToF-MS). The concentration of m/z 45.031 (t.i. acetaldehyde) was significantly (p < 0.05) higher after 7 days of fermentation by LP100 in the DM supplemented with threonine compared to all other media fermented by all three strains. The concentrations of m/z 49.012 (t.i. methanethiol) and m/z 95.000 (t.i. dimethyl disulfide) were significantly (p < 0.05) higher after 7 days of fermentation by either LP100, PP100, or LB672 in the DM supplemented with methionine compared to all other media. Information on the role of individual AAs on VOCs generation by different LAB strains will help to guide flavour development from the fermentation of plant-based substrates.

Abstract Volatile organic compounds (VOCs) might mediate microbial interactions, especially in spatially structured environments, such as soil. However, the variety and specificity of VOC production are poorly understood. Here, we studied 25 Mortierellaceae strains belonging to the genera Linnemannia and Entomortierella in both pure and co-culture with Pseudomonas helmanticensis under laboratory conditions. We analysed both the fungal growth depending on co-cultivation and the cultures’ volatilomes applying proton-transfer-reaction time-of-flight and gas chromatography-mass spectrometry (PTR-ToF-MS and GC–MS). In a strain-specific manner, we found the fungi’s radial growth rate and colony morphology affected by the presence of P. helmanticensis. The fungus seemed to generally reduce the bacterial growth. The volatilomes of the fungal and bacterial pure and co-cultures were diverse. While the fungi frequently consumed VOCs, P. helmanticensis produced a higher diversity and amount of VOCs than any fungal strain. Our results support that both the pure and co-culture volatilomes are taxonomically conserved. Taken together, our data supports the relevance of VOCs in Mortierellaceae-P. helmanticensis interaction. We also discuss individual VOCs that appear relevant in the interaction.

The low temperature normally applied to prevent fruit decay during the storage of apples, can also triggers the onset of a chilling injury disorder known as superficial scald. In this work, the etiology of this disorder and the mechanism of action of two preventing strategies, such as the application of 1-MCP (1-methylcyclopropene) and storage at low oxygen concentration in ‘Granny Smith’ and ‘Ladina’ apple cultivars were investigated. The metabolite assessment highlighted a reorganization of specific metabolites, in particular flavan-3-ols and unsaturated fatty acids, while the genome-wide transcriptomic analysis grouped the DEGs into four functional clusters. The KEGG pathway and GO enrichment analysis, together with the gene-metabolite interactome, showed that the treatment with 1-MCP prevented the development of superficial scald by actively promoting the production of unsaturated fatty acids, especially in ‘Granny Smith’. ‘Ladina’, more susceptible to superficial scald and less responsive to the preventing strategies, was instead characterized by a higher accumulation of very long chain fatty acids. Storage at low oxygen concentration stimulated a higher accumulation of ethanol and acetaldehyde together with the expression of genes involved in anaerobic respiration, such as malate, alcohol dehydrogenase and pyruvate decarboxylase in both cultivars. Low oxygen concentration, likewise 1-MCP, through a direct control on ethylene prevented the onset of superficial scald repressing the expression of PPO, a gene encoding for the polyphenol oxidase enzyme responsible of the oxidation of chlorogenic acid. Moreover, in ‘Granny Smith’ apple, the expression of three members of the VII subgroups of ERF genes, encoding for elements coordinating the acclimation process to hypoxia in plants was observed. The global RNA-Seq pattern also elucidated a specific transcriptomic signature between the two cultivars, disclosing the effect of the different genetic background in the control of this disorder.

The application of direct-injection mass spectrometric (DI-MS) techniques, like Proton Transfer Reaction Time of Flight Mass Spectrometry (PTR-ToF-MS) has been suggested as a reliable phenotyping tool for fruit volatilome assessment in both genetic and quality-related studies. In this study the complexity of raspberry aroma was investigated by a comprehensive untargeted VOC analysis, done by combining SPME-GC-MS and PTR-ToF-MS assessments with multi-block discriminant analysis using the DIABLO mixOmics framework. The aim was to acquire an exhaustive characterization of the raspberry volatilome according to different fruit ripening stages (pink, ripe, and overripe) and genetic variances (50 accessions), as well as to investigate the potential of PTR-ToF-MS as a rapid and high throughput VOC phenotyping tool to address issues related to raspberry fruit quality. Results of this study demonstrated the complementarity between SPME-GC-MS and PTR-ToF-MS techniques to evaluate the raspberry aroma composition. PTR-ToF-MS generates reliable raspberry VOC fingerprints mainly due to a reduced compound fragmentation and precise content estimation. In addition, the high collinearity between isomers of monoterpenes and norisoprenoids, discovered by GC analysis, reduces the main analytic limitation of PTR-ToF-MS of not being able to separate isomeric molecules. The high similarity between the VOC matrices obtained by applying PTR-ToF-MS and SPME-GC-MS confirmed the possibility of using PTR-ToF-MS as a reliable high throughput phenotyping tool for raspberry volatiolome assessment. In addition, results provided by the germplasm collection investigation enabled to distinguish the best performing accessions, based on VOCs composition, to be used as superior parental lines for future breeding programs.

The impact of the ethylene inhibitor, 1-methylcyclopropene (1-MCP), on four apple cultivars (Braeburn, Fuji, Jazz and Golden Delicious) over 150 days of storage at 2 °C was assessed. Proton transfer reaction quadrupole mass spectrometry (PTR-QUAD-MS) was used to monitor changes in VOC composition, while texture analysis and X-ray microcomputer tomography (µ-CT) scanning were used to study microstructural changes. The application of 1-MCP on apples reduced VOC emissions, concurrently maintaining a firmer texture compared to the untreated apples at each time point. The µ-CT scanning revealed how changes in specific morphological characteristics such as anisotropy, connectivity and porosity, size and shape, as well as the interconnectivity of intracellular spaces (IS) influenced texture even when porosity was similar. Additionally, this study showed that the porosity and connectivity of IS were associated with VOC emission and increased simultaneously. This study highlights how the morphological parameters of an apple can help explain their ripening process during long-term storage and how their microstructure can influence the release of VOCs.

Direct injection mass spectrometry (DIMS) entails the direct introduction of a gaseous sample into a mass analyser without prior treatment or separation. DIMS techniques offer the opportunity to monitor processes in time, with limits of detection as low as 0.5 parts per trillion in volume (for a 1 s measurement time) while providing results with high informational content. This review provides insight into current and promising future developments of DIMS in the analysis of grape, wine and other alcoholic beverages. Thanks to its unique characteristics, DIMS allows the online monitoring of volatile organic compounds (VOCs) released by grapes during fermentative bioprocesses or by wine directly from the glass headspace or during drinking. A DIMS-based approach can also be adopted to perform quality control and high-throughput analysis, allowing us to characterise the volatile profile of large sample sets rapidly and in a comprehensive fashion. Furthermore, DIMS presents several characteristic elements of green analytical chemistry approaches, catalysing an interest linked to the development of sustainable paths in research and development activities in the field of viticulture and oenology.

Volatile organic compounds (VOCs) are molecules present in our everyday life, and they can be positive, such as in the formation of odour and food flavour, or harmful to the environment and humans, and research is focusing on limiting their emissions. Various methods have been used to achieve this purpose. Firstly, we review three main degradation methods: activated carbon, photocatalysis and a synergetic system. We provide a general overview of the operative conditions and report the possibility of VOC abatement during cooking. Within the literature, none of these systems has ever been tested in the presence of complex matrices, such as during cooking processes. The aim of this study is to compare the three methods in order to understand the behaviour of filter systems in the case of realistically complex gas mixtures. Proton transfer reaction–mass spectrometry (PTR-MS) has been used in the real-time monitoring of volatilome. Due to the fact that VOC emissions are highly dependent on the composition of the food cooked, we evaluated the degradation capacity of the three systems for different burger types (meat, greens, and fish). We demonstrate the pros and cons of photocatalysis and adsorption and how a combined approach can mitigate the drawbacks of photocatalysis.

The capacity to emit isoprene, among other stresses, protects plants from drought, but the molecular mechanisms underlying this trait are only partly understood. The Arecaceae (palms) constitute a very interesting model system to test the involvement of isoprene in enhancing drought tolerance, as their high isoprene emissions may have contributed to make them hyperdominant in neotropical dry forests, characterized by recurrent and extended periods of drought stress. In this study we isolated and functionally characterized a novel isoprene synthase, the gene responsible for isoprene biosynthesis, from Copernicia prunifera, a palm from seasonally dry tropical forests. When overexpressed in the non-emitter Arabidopsis thaliana, CprISPS conferred significant levels of isoprene emission, together with enhanced tolerance to water limitation throughout plant growth and development, from germination to maturity. CprISPS overexpressors displayed higher germination, cotyledon/leaf greening, water usage efficiency, and survival than WT Arabidopsis under various types of water limitation. This increased drought tolerance was accompanied by a marked transcriptional up-regulation of both ABA-dependent and ABA-independent key drought response genes. Taken together, these results demonstrate the capacity of CprISPS to enhance drought tolerance in Arabidopsis and suggest that isoprene emission could have evolved in Arecaceae as an adaptive mechanism against drought.

Proton transfer reaction mass spectrometry (PTR-MS) has been developed for the direct, high sensitivity and high time resolution monitoring of volatile organic compounds (VOCs). Although PTR-MS development was not guided by greenness goals, most of its features perfectly fit within the green analytical chemistry (GAC) principles, making PTR-MS an intrinsically green analytical technique. Indeed, in its basic implementation, it does not require solvents or non-renewable carrier gases and, in principle, distilled water, used to feed the source where precursors ions are formed, is the only consumable.Food science and technology and agroindustry are amongst the fields where PTR-MS has been successfully exploited. Here we review and discuss, with emphasis on the GAC requirements, the potential of PTR-MS as a tool for both fundamental research and industrial applications in different food-related themes: i) food consumption and sensory, ii) bioprocess monitoring, iii) traceability, iv) quality control, and v) high-throughput food volatilome phenotyping.The outcome of all these related studies indicates PTR-MS both as a complementary tool to gas chromatographic methods and as a valuable technique when reduced analysis time, high sensitivity and/or on-line measurement are required.

Hop-derived volatile organic compounds (VOCs) and their transformation products significantly impact beer flavour and aroma. Geraniol, a key monoterpene alcohol in hops, has been reported to undergo yeast-modulated biotransformation into various terpenoids during fermentation, which impacts the citrus and floral aromas of the finished beer. This study monitored the evolution of geraniol and its transformation products throughout fermentation to provide insight into differences as a function of yeast species and strain. The headspace concentration of VOCs produced during fermentation in model wort was measured using Solid-Phase Microextraction Gas Chromatography/Mass Spectrometry (SPME-GC/MS) and Proton Transfer Reaction-Time of Flight-Mass Spectrometry (PTR-ToF-MS). In the absence of yeast, only geraniol was detected, and no terpenoid compounds were detected in geraniol-free ferments. During fermentation, the depletion of geraniol was closely followed by the detection of citronellol, citronellyl acetate and geranyl acetate. The concentration of the products and formation behaviour was yeast strain dependent. SPME-GC/MS provided confidence in compound identification. PTR-ToF-MS allowed online monitoring of these transformation products, showing when formation differed between Saccharomyces cerevisiae and Saccharomyces pastorianus yeasts. A better understanding of the ability of different yeast to biotransform hop terpenes will help brewers predict, control, and optimize the aroma of the finished beer.

Ethylene, produced endogenously by plants and their organs, can induce a wide array of physiological responses even at very low concentrations. Nevertheless, the role of ethylene in regulating blueberry (Vaccinium spp.) ripening and storability is still unclear although an increase in ethylene production has been observed in several studies during blueberry ripening. To overcome this issue, we evaluated the endogenous ethylene production of a Vaccinium germplasm selection at different fruit ripening stages and after cold storage, considering also textural modifications. Ethylene and texture were further assessed also on a bi-parental full-sib population of 124 accessions obtained by the crossing between “Draper” and “Biloxi”, two cultivars characterized by a different chilling requirement and storability performances. Our results were compared with an extensive literature research, carried out to collect all accessible information on published works related to Vaccinium ethylene production and sensitivity. Results of this study illustrate a likely role of ethylene in regulating blueberry shelf life. However, a generalisation valid for all Vaccinium species is not attainable because of the high variability in ethylene production between genotypes, which is strictly genotype-specific. These differences in ethylene production are related with blueberry fruit storage performances based on textural alterations. Specifically, blueberry accessions characterized by the highest ethylene production had a more severe texture decay during storage. Our results support the possibility of tailoring ad hoc preharvest and postharvest strategies to extend blueberry shelf life and quality according with the endogenous ethylene production level of each cultivar.

Gas sensors play an important role in many areas of human life, including the monitoring of production processes, occupational safety, food quality assessment, and air pollution monitoring. Therefore, the need for gas sensors to monitor hazardous gases, such as ammonia, at low operating temperatures has become increasingly important in many fields. Sensitivity, selectivity, low cost, and ease of production are crucial characteristics for creating a capillary network of sensors for the protection of the environment and human health. However, developing gas sensors that are not only efficient but also small and inexpensive and therefore integrable into everyday life is a difficult challenge. In this paper, we report on a resistive sensor for ammonia detection based on thin V2O5 nanosheets operating at room temperature. The small thickness and porosity of the V2O5 nanosheets give the sensors good performance for sensing ammonia at room temperature (RT), with a relative change of resistance of 9.4% to 5 ppm ammonia (NH3) and an estimated detection limit of 0.4 ppm. The sensor is selective with respect to the seven interferents tested; it is repeatable and stable over the long term (four months). Although V2O5 is generally an n-type semiconductor, in this case the nanosheets show a p-type semiconductor behavior, and thus a possible sensing mechanism is proposed. The device’s performance, along with its size, low cost, and low power consumption, makes it a good candidate for monitoring freshness and spoilage along the food supply chain.

Meat flavor is an important aspect of meat quality that also influences consumer demand, and is therefore very important for the meat industry. Volatile organic compounds (VOCs) contribute in large part to the flavor of meat, and while increasing numbers of articles are published on this topic, reviews of these articles are very scarce. Therefore, our aim was to perform a bibliometric analysis of the scientific publications on VOCs in meat over the period 2000–2020. We selected 611 scientific sources from the Scopus database related to VOCs in meat (seafood excluded). The bibliometric information retrieved included journals, authors, countries, institutions, keywords, and citations. From this analysis, we drew up a list of the most important journals, authors, countries, and institutions, and the trends in VOC research on meat. We conducted a social network analysis (SNA) to identify the collaborations among the many authors and countries, and a keyword analysis to generate a network map of the authors’ keywords. We also determined which meat species were most frequently chosen as research subjects, traced the evolution of the various methods/instruments used, and explored the research tendencies. Finally, we point out the need for further research in defining meat quality, improving meat flavor, identifying adulterants, and certifying the authenticity of meat.

This work presents in vitro and in vivo aroma release analysis of three espresso coffees carried out by PTR-ToF-MS headspace and nosespace analysis, respectively. The products were C. arabica coffees prepared using an espresso coffee machine: a low-caffeine C. arabica var. laurina light roast, a low-caffeine C. arabica var. laurina dark roast, and a single-origin coffee from Ethiopia which were roasted to a medium roast degree. Headspace analysis allowed for discrimination between coffees with a prediction accuracy of 92% or higher. Relevant discriminating compounds were related to the roasting degree and varietal compounds. Coffee nosespace consisted of 35 mass peaks overall. Despite this relatively low number of detected peaks, coffee discrimination was still possible with ≥93% accuracy. The compounds most relevant to the discrimination were those related to the roasting degree. Major differences—both qualitative and quantitative—were found between headspace and nosespace profiles.

Juglans regia (L.) is cultivated worldwide for its nutrient-rich nuts. In Italy, despite the growing demand, walnut cultivation has gone through a strong decline in recent decades, which led to Italy being among the top five net importing countries. To promote the development of local high-quality Italian walnut production, we devised a multidisciplinary project to highlight the distinctive traits of three varieties grown in the mountainous region Trentino (northeast of Italy): the heirloom ‘Bleggiana’, a second local accession called local Franquette and the French cultivar ‘Lara’, recently introduced in the local production to increase yield. The genetic characterization confirmed the uniqueness of ‘Bleggiana’ and revealed local Franquette as a newly described autochthonous variety, thus named ‘Blegette’. The metabolic profiles highlighted a valuable nutritional composition of the local varieties, richer in polyphenols and with a lower ω-6/ω-3 ratio than the commercial ‘Lara’. ‘Blegette’ obtained the highest preference scores from consumers for both the visual aspect and tasting; however, the volatile organic compound profiles did not discriminate among the characterized cultivars. The described local varieties represent an interesting reservoir of walnut genetic diversity and quality properties, which deserve future investigation on agronomically useful traits (e.g., local adaptation and water usage) for a high-quality and sustainable production.

Methanol, naturally present in small quantities in the distillation of alcoholic beverages, can lead to serious health problems. When it exceeds a certain concentration, it causes blindness, organ failure, and even death if not recognized in time. Analytical techniques such as chromatography are used to detect dangerous concentrations of methanol, which are very accurate but also expensive, cumbersome, and time-consuming. Therefore, a gas sensor that is inexpensive and portable and capable of distinguishing methanol from ethanol would be very useful. Here, we present a resistive gas sensor, based on tin oxide nanowires, that works in a thermal gradient. By combining responses at various temperatures and using machine learning algorithms (PCA, SVM, LDA), the device can distinguish methanol from ethanol in a wide range of concentrations (1–100 ppm) in both dry air and under different humidity conditions (25–75% RH). The proposed sensor, which is small and inexpensive, demonstrates the ability to distinguish methanol from ethanol at different concentrations and could be developed both to detect the adulteration of alcoholic beverages and to quickly recognize methanol poisoning.