Search

In this perspective article, several internationally recognized experts, members of the editorial team of this journal, discuss a selection of current hot topics identified in Food Science and Foodomics. The topics are comprised of the main areas of Food Science and Foodomics, namely, food safety, food authenticity, food processing, and food bioactivity. Logically, several of the discussed topics involve more than one of the mentioned main areas. Regarding food safety, the topics discussed are the use of analytical nanotechnology, nanometrology, nano-chromatography; the determination of organic contaminants based on MS and NMR; the impact of microplastics and nanoplastics on food or the contamination of foods with plant toxins. Regarding food authenticity, the paper discusses the role of MS, NMR, biosensors and the new trends in foodomics for food authentication. In terms of food processing, the work shows interesting perspectives on novel processing technologies, the effect of food processing on the gut microbiota or in the interaction among secondary metabolites and macromolecules; the development of active packaging, and the potential effects of introducing recycled plastics in food packaging; the new green extraction and encapsulation strategies of bioactive compounds from food by-products; and the anti-biofilm capacity of natural compounds/extracts/vegetal oils and essential oils. Food bioactivity and the relation between food and health includes the bioavailability and bioaccessibility of bioactive compounds; new trends and challenges in the interaction of nutraceuticals with biological systems; how food matrix impacts the bioaccessibility of nutrients and bioactive compounds; or the study of biodiversity, food and human health through one-health concept. We anticipate elaborations on these hot topics will promote further studies in Food Science and Foodomics.

The aim of this study was to evaluate the metabolomic profile of T. molitor larvae reared on the following innovative growth substrates: wheat bran (control, CTRL); wheat bran supplemented with 12.5% w/w chestnut shell (TRT1); and wheat bran supplemented with 25% w/w chestnut shell (TRT2) for 14 days of trial. At the end of this experiment, larvae were transformed into insect meals for nutritional characterization. Nuclear Magnetic Resonance (NMR) spectroscopy was carried out to evaluate the metabolomic profile of organic acids, sugars, nitrogen bases and derivates, fatty acids, and other compounds. Chemical analysis showed an increased level of crude protein in TRT1 compared to CTRL and TRT2 (p = 0.0391). The metabolite profiles of TRT1 and TRT2 were similar to each other but distinct from those of the CTRL group. Notably, larvae enriched with chestnut shells revealed the presence of uracil, uridine, and glucose, while fumarate was absent. The enrichment analysis showed that in TRT1 and TRT2, the glyoxylate and dicarboxylate metabolism was more relevant compared to CTRL. These findings indicate that chestnut shell inclusion affects the larvae metabolism of T. molitor and demonstrates the effectiveness of NMR spectroscopy in revealing a relation between insect metabolism and growth substrate.

Food reformulation is a strategy to make healthier foods by using food waste matrices that are still nutritionally valid. A shortbread cookie was reformulated replacing hazelnut skin (HS) of the Tonda Gentile Romana variety (5% and 10%) to refined flour and proportionally decreasing the butter amount. This resulted in significant, two- and five-fold, increases in the antioxidant capacity compared with the control, in the 5% and 10% fortified recipes, respectively. Among the most important antioxidants, gallic acid, catechin, phloridzin, and protocatechuic acid were found. Moreover, here we found, for the first time, that HS from the Romana variety had a high total fiber content (44.13 g/100 g), most of which was insoluble fiber. Therefore, HS 10% addition to the shortbread cookie recipe caused a significant increase in fiber content, making the experimental cookie earn the nutritional claim of “high fiber content”. Finally, preliminary evidence demonstrated that 10% HS, in comparison to 5%, following in vitro upper gastrointestinal digestion, conferred significant prebiotic activity in an in vitro culture of L. rhamnosus. Therefore, from the perspective of the circular economy, HS could be a valuable ingredient to increase the antioxidant and prebiotic activities of conventional foods.

Officinal plants are a source of metabolites whose chemical composition depends on pedoclimatic conditions. In this study, the NMR-based approach was applied to investigate the impacts of different altitudes and agronomical practices (Land, Mountain Spontaneous, and Organically Grown Ecotypes, namely LSE, MSE, and OE, respectively) on the metabolite profiles of Burdock root, Dandelion root and aerial part, and Lemon balm aerial part. Sugars, amino acids, organic acids, polyphenols, fatty acids, and other metabolites were identified and quantified in all samples. Some metabolites turned out to be tissue-specific markers. Arginine was found in roots, whereas myo-inositol, galactose, glyceroyldigalactose moiety, pheophytin, and chlorophyll were identified in aerial parts. Caftaric and chicoric acids, 3,5 di-caffeoylquinic acid, and chlorogenic and rosmarinic acids were detected in Dandelion, Burdock and Lemon balm, respectively. The metabolite amount changed significantly according to crop, tissue type, and ecotype. All ecotypes of Burdock had the highest contents of amino acids and the lowest contents of organic acids, whereas an opposite trend was observed in Lemon balm. Dandelion parts contained high levels of carbohydrates, except for the MSE aerial part, which showed the highest content of organic acids. The results provided insights into the chemistry of officinal plants, thus supporting nutraceutical–phytopharmaceutical research.

Hemp bioproducts hold great promise as valuable materials for nutraceutical and pharmaceutical applications due to their diverse bioactive compounds and potential health benefits. In line with this interest and in an attempt to valorize the Lazio Region crops, this present study investigated chemically characterized hydroalcoholic and organic extracts, obtained from the inflorescences of locally cultivated Felina 32, USO 31, Ferimon and Fedora 17 hemp varieties. In order to highlight the possible chemopreventive power of the tested samples, a bioactivity screening was performed, which included studying the antimutagenic activity, radical scavenging power, cytotoxicity in human hepatoma HepG2 cells, leakage of lactate dehydrogenase (LDH) and modulation of the oxidative stress parameters and glucose-6-phosphate dehydrogenase (G6PDH) involved in the regulation of the cell transformation and cancer proliferation. Tolerability studies in noncancerous H69 cholangiocytes were performed, too. The organic extracts showed moderate to strong antimutagenic activities and a marked cytotoxicity in the HepG2 cells, associated with an increased oxidative stress and LDH release, and to a G6PDH modulation. The hydroalcoholic extracts mainly exhibited radical scavenging properties with weak or null activities in the other assays. The extracts were usually well-tolerated in H69 cells, except for the highest concentrations which impaired cell viability, likely due to an increased oxidative stress. The obtained results suggest a possibility in the inflorescences from the Felina 32, USO 31, Ferimon and Fedora 17 hemp varieties as source of bioactive compounds endowed with genoprotective and chemopreventive properties that could be harnessed as preventive or adjuvant healing strategies.

Beauvericin (BEA) is an emerging mycotoxin produced by some species of Fusarium genera that widely contaminates food and feed. Gentiana lutea is a protected medicinal plant known for its antioxidant and anti-inflammatory properties, which are attributed to its rich content of bioactive compounds. In order to evaluate the beneficial effects of G. lutea flower against BEA cytotoxicity, the aim of this study is to evaluate changes in protein expression after Jurkat cell exposure through a proteomics approach. To carry out the experiment, cells were exposed to intestinally digested G. lutea flower alone or in combination with the BEA standard (100 nM) over 7 days. Differentially expressed proteins were statistically evaluated (p < 0.05), revealing a total of 172 proteins with respect to the control in cells exposed to the BEA standard, 145 proteins for G. lutea alone, and 139 proteins when exposing the cells to the combined exposure. Bioinformatic analysis revealed processes implicated in mitochondria, ATP-related activity, and RNA binding. After careful analysis of differentially expressed proteins, it was evident that G. lutea attenuated, in most cases, the negative effects of BEA. Furthermore, it decreased the presence of major oncoproteins involved in the modulation of immune function.

Wood Decay Fungi (WDF) are fungi specialized in degrading wood. An interesting perspective is their use as a source of Novel Foods or food ingredients. Here, for the first time, the metabolite profiling of hydroalcoholic and organic extracts from A. biennis, F. iberica, S. hirsutum mycelia was investigated by NMR methodology. Amino acids (alanine, arginine, asparagine, aspartate, betaine, GABA, glutamate, glutamine, histidine, isoleucine, leucine, lysine, phenylalanine, threonine, tryptophan, tyrosine, valine), sugars (galactose, glucose, maltose, trehalose, mannitol), organic acids (acetate, citrate, formate, fumarate, lactate, malate, succinate), adenosine, choline, uracil and uridine were identified and quantified in the hydroalcoholic extracts, whereas the 1H spectra of organic extracts showed the presence of saturated, mono-unsaturated and di-unsaturated fatty chains, ergosterol,1,2-diacyl-sn-glycero-3-phosphatidylethanolamine, and 1,2-diacyl-sasglycero-3-phosphatidylcholine. A. biennis extracts showed the highest amino acid concentration. Some compounds were detected only in specific species: betaine and mannitol in S. hirsutum, maltose in A. biennis, galactose in F. iberica, GABA in F. iberica and S. hirsutum, and acetate in A. biennis and S. hirsutum. S. hirsutum showed the highest saturated fatty chain concentration, whereas DUFA reached the highest concentration in A. biennis. A high amount of ergosterol was measured both in A. biennis and F. iberica. The reported results can be useful in the development of WDF-based products with a high nutritional and nutraceutical value.

Acheta domesticus (house cricket) has been recently introduced into the official European list of novel foods, representing an alternative and sustainable food source. Up to now, the chemical characterization of this edible insect has been focused only on specific classes of compounds. Here, three production batches of an A. domesticus powder were investigated by means of a multimethodological approach based on NMR, FT-ICR MS, and GC-MS methodologies. The applied analytical protocol, proposed for the first time in the study of an edible insect, allowed us to identify and quantify compounds not previously reported in crickets. In particular, methyl-branched hydrocarbons, previously identified in other insects, together with other compounds such as citrulline, formate, γ-terpinene, p-cymene, α-thujene, β-thujene, and 4-carene were detected. Amino acids, organic acids, and fatty acids were also identified and quantified. The improved knowledge of the chemical profile of this novel food opens new horizons both for the use of crickets as a food ingredient and for the use of extracts for the production of new formulations. In order to achieve this objective, studies regarding safety, biological activity, bioaccessibility, and bioavailability are needed as future perspectives in this field.

The recovery of bioactive compounds from crop byproducts leads to a new perspective way of waste reutilization as a part of the circular economy. The present study aimed at an exhaustive metabolite profile characterization of globe artichoke and cauliflower byproducts (leaves, stalks, and florets for cauliflower only) as a prerequisite for their valorization and future implementations. The metabolite profile of aqueous and organic extracts of byproducts was analyzed using the NMR-based metabolomics approach. Free amino acids, organic acids, sugars, polyols, polyphenols, amines, glucosinolates, fatty acids, phospho- and galactolipids, sterols, and sesquiterpene lactones were identified and quantified. In particular, globe artichoke byproducts are a source of health-beneficial compounds including chiro-inositol (up to 10.1 mg/g), scyllo-inositol (up to 1.8 mg/g), sesquiterpene lactones (cynaropicrin, grosheimin, dehydrocynaropicrin, up to 45.5 mg/g in total), inulins, and chlorogenic acid (up to 7.5 mg/g), whereas cauliflower byproducts enclose bioactive sulfur-containing compounds S-methyl-L-cysteine S-oxide (methiin, up to 20.7 mg/g) and glucosinolates. A variable content of all metabolites was observed depending on the crop type (globe artichoke vs. cauliflower) and the plant part (leaves vs. stalks). The results here reported can be potentially used in different ways, including the formulation of new plant biostimulants and food supplements.

Insects, especially crickets, have been proposed as a novel source of nutrients in human nutrition since they possess bioactive molecules, including high protein content, lipids, chitin, vitamins and minerals. In this work, the nutritional and functional properties of a novel Italian spray-dried (SD) cricket powder were evaluated. The powder was characterized by physico–chemical properties (morphology, size distribution, solid state, thermal profiles, and surface zeta potential), and antioxidant properties. Moreover, preclinical properties (cytocompatibility and pro-inflammatory immune response) were assessed. The powder was characterized by microparticle structure with bulges and rough surfaces, showing distinctive antioxidant properties. The preclinical results suggested that the SD crickets were biocompatible towards Caco-2 and macrophages without immune response, representing an interesting material for the food industry that could provide health benefits in addition to the basic nutritional value of traditional foods.

In this study, the effect of several agronomical practices on the chemical composition of hemp inflorescences, a potential novel food that needs to be further studied, was observed. Here, the case study of inflorescences from Ferimon cultivars is discussed and submitted to different agronomical practices (irrigation and fertilizers) in different years, and the inflorescences harvested in different periods were analyzed by a multimethodological approach. Targeted and untargeted methodologies allowed cannabinoids, total phenolic content, metabolite profile and antioxidant activity to be determined. The biomass and inflorescence yields were also reported. The whole data set was submitted to ANOVA-simultaneous component analysis. The statistic results allowed us to observe that irrigation was responsible for the (–)-Δ9-tetrahydrocannabinol (THC) and cannabidiol (CBD) increment. THC, cannabichromene (CBC), cannabigerol (CBG), succinate, and fructose resulted as higher in full female flowering than in the period of seed maturity. On the other hand, nitrogen supplementation led to an increase of iso-leucine, valine, and threonine. The obtained results underlined both the potential food application of hemp inflorescences, due to the rich chemical profile, and the strong effect of agronomical practices, mainly irrigation and harvesting, on the qualitative and quantitative characteristics of its metabolite profile.

In this review, the three different NMR-based approaches usually used to study foodstuffs are described, reporting specific examples. The first approach starts with the food of interest that can be investigated using different complementary NMR methodologies to obtain a comprehensive picture of food composition and structure; another approach starts with the specific problem related to a given food (frauds, safety, traceability, geographical and botanical origin, farming methods, food processing, maturation and ageing, etc.) that can be addressed by choosing the most suitable NMR methodology; finally, it is possible to start from a single NMR methodology, developing a broad range of applications to tackle common food-related challenges and different aspects related to foods.

The application of Nuclear Magnetic Resonance in food science has grown exponentially over the past few decades [...]

Semen cryopreservation represents the main tool for preservation of biodiversity; however, in avian species, the freezing–thawing process results in a sharp reduction in sperm quality and consequently fertility. Thus, to gain a first insight into the molecular basis of the cryopreservation of turkey sperm, the NMR-assessed metabolite profiles of fresh and frozen–thawed samples were herein investigated and compared with sperm qualitative parameters. Cryopreservation decreased the sperm viability, mobility, and osmotic tolerance of frozen–thawed samples. This decrease in sperm quality was associated with the variation in the levels of some metabolites in both aqueous and lipid sperm extracts, as investigated by NMR analysis. Higher amounts of the amino acids Ala, Ile, Leu, Phe, Tyr, and Val were found in fresh than in frozen–thawed sperm; on the contrary, Gly content increased after cryopreservation. A positive correlation (p < 0.01) between the amino acid levels and all qualitative parameters was found, except in the case of Gly, the levels of which were negatively correlated (p < 0.01) with sperm quality. Other water-soluble compounds, namely formate, lactate, AMP, creatine, and carnitine, turned out to be present at higher concentrations in fresh sperm, whereas cryopreserved samples showed increased levels of citrate and acetyl-carnitine. Frozen–thawed sperm also showed decreases in cholesterol and polyunsaturated fatty acids, whereas saturated fatty acids were found to be higher in cryopreserved than in fresh sperm. Interestingly, lactate, carnitine (p < 0.01), AMP, creatine, cholesterol, and phosphatidylcholine (p < 0.05) levels were positively correlated with all sperm quality parameters, whereas citrate (p < 0.01), fumarate, acetyl-carnitine, and saturated fatty acids (p < 0.05) showed negative correlations. A detailed discussion aimed at explaining these correlations in the sperm cell context is provided, returning a clearer scenario of metabolic changes occurring in turkey sperm cryopreservation.

In present study, the potential functional properties of the ethanolic extracts from peel, pulp, edible part and seeds of Capsicum annuum L. var. Cornetto di Pontecorvo were studied. The antimutagenicity against environmental pollutants and oxidative mutagens, the digestive enzyme inhibition, and the antioxidant properties were evaluated in relation to phenolic content. All the samples produced antimutagenic effects against 1-nitropyrene, 2-aminoantracene and tert-butyl-hydroperoxide, and inhibited α-amylase, without affecting α-glucosidase. Also, radical scavenging effects, inhibition of ROS-mediated lipoperoxidation and chelating activity were highlighted. The peel and seed extracts were in general the most effective samples. The phytochemical analysis highlighted a high amount of polyphenols, with a very low carotenoid content. Among phenolics, rutin, gallic acid, carvacrol, chlorogenic acid, 4-OH benzoic acid, and traces of quercetin and epicatechin were determined. Present results highlight a functional role of this pepper ecotype and suggest a possible use of its derived products as food supplements.

Cannabis sativa L. crops have been traditionally exploited as sources of fibers, nutrients, and bioactive phytochemicals of medical interest. In the present study, two terpene-rich organic extracts, namely FOJ and FOS, obtained from Felina 32 hemp inflorescences collected in June and September, respectively, have been studied for their in vitro anticancer properties. Particularly, their cytotoxicity was evaluated in different cancer cell lines, and the possible entourage effect between nonintoxicating phytocannabinoids (cannabidiol and cannabichromene) and caryophyllane sesquiterpenes (β-caryophyllene, β-caryophyllene oxide and α-humulene), as identified at GC/MS analysis, was characterized. Modulation of cannabinoid CB1 and CB2 receptors was studied as a mechanistic hypothesis. Results highlighted marked cytotoxic effects of FOJ, FOS, and pure compounds in triple negative breast cancer MDA-MB-468 cells, likely mediated by a CB2 receptor activation. Cannabidiol was the main cytotoxic constituent, although low levels of caryophyllane sesquiterpenes and cannabichromene induced potentiating effects; the presence in the extracts of unknown antagonistic compounds has been highlighted too. These results suggest an interest in Felina 32 hemp inflorescences as a source of bioactive phytocomplexes with anticancer properties and strengthen the importance of considering the possible involvement of minor terpenes, such as caryophyllane sesquiterpenes, in the entourage effect of hemp-based extracts.

A multidisciplinary protocol is proposed to monitor the preservation of fresh pumpkin samples (FP) using three commercial polymeric films: A made of biodegradable cellophane from regenerated cellulose pulp; B from corn starch, cassava and eucalyptus, C made of polylactic acid from corn starch, and a polyethylene film used as reference (REF). Chemical, mechanical and microbiological analyses were applied on packaging and fresh and packaged samples at different times. After an 11-day period, NMR spectroscopy results showed a sucrose increase and a malic acid decrease in all the biofilms with respect to FP; fructose, glucose, galactose levels remained quite constant in biofilms B and C; the most abundant amino acids remained quite constant in biofilm A and decreased significantly in biofilm B. From microbiological analyses total microbial count was below the threshold value up to 7 days for samples in all the films, and 11 days for biofilm C. The lactic acid bacteria, and yeasts and molds counts were below the acceptability limit during the 11 days for all packages. In the case of biofilm C, the most promising packaging for microbiological point of view, aroma analysis was also carried out. In this paper, you can find all the analysis performed and all the values found.

The metabolite profile of fresh Goji berries from two cultivars, namely Big Lifeberry (BL) and Sweet Lifeberry (SL), grown in the Lazio region (Central Italy) and harvested at two different periods, August and October, corresponding at the beginning and the end of the maturation, was characterized by means of nuclear magnetic resonance (NMR) and electrospray ionization Fourier transform ion cyclotron resonance (ESI FT-ICR MS) methodologies. Several classes of compounds such as sugars, amino acids, organic acids, fatty acids, polyphenols, and terpenes were identified and quantified in hydroalcoholic and organic Bligh-Dyer extracts. Sweet Lifeberry extracts were characterized by a higher content of sucrose with respect to the Big Lifeberry ones and high levels of amino acids (glycine, betaine, proline) were observed in SL berries harvested in October. Spectrophotometric analysis of chlorophylls and total carotenoids was also carried out, showing a decrease of carotenoids during the time. These results can be useful not only to valorize local products but also to suggest the best harvesting period to obtain a product with a chemical composition suitable for specific industrial use. Finally, preliminary studies regarding both the chemical characterization of Goji leaves generally considered a waste product, and the biological activity of Big Lifeberry berries extracts was also investigated. Goji leaves showed a chemical profile rich in healthy compounds (polyphenols, flavonoids, etc.) confirming their promising use in the supplements/nutraceutical/cosmetic field. MG63 cells treated with Big Lifeberry berries extracts showed a decrease of iNOS, COX-2, IL-6, and IL-8 expression indicating their significant biological activity.

Untargeted (NMR) and targeted (RP-HPLC-PDA-ESI-MSn, RP-HPLC-FD) analytical methodologies were used to determine the bioactive components of 19 tea samples, characterized by different production processes (common tea and GABA tea), degrees of fermentation (green and oolong teas), and harvesting season (autumn and spring). The combination of NMR data and a multivariate statistical approach led to a statistical model able to discriminate between GABA and non-GABA teas and green and oolong teas. Targeted analyses showed that green and GABA green teas had similar polyphenol and caffeine contents, but the GABA level was higher in GABA green teas than in regular green tea samples. GABA oolong teas showed lower contents of polyphenols, caffeine, and amino acids, and a higher content of GABA, in comparison with non-GABA oolong teas. In conclusion, the results of this study suggest that the healthy properties of teas, especially GABA teas, have to be evaluated via comprehensive metabolic profiling rather than only the GABA content.

Abstract Background The quality grade of an olive oil is defined according to the results of analytical and organoleptic examinations.The increasing attention towards both olive oil quality and quality verification methods prompted us to undertake a “critical” analysis of analytical and sensory data supplied by an International Certificated Body (ICB), relative to commercial olive oils produced in Mediterranean areas and purchased in Italy and in USA. Methods ICB data included chemical analyses namely free acidity, peroxide index, spectrophotometric UV evaluation, fatty acid ethyl esters and stigmadiens content and organoleptic evaluations carried out by nine official International Olive Council labs according to EEC Regulation 2568/91. Results The results of the chemical analyses, except the fatty acid ethyl ester content, obtained from the nine labs were consistent giving rise to the same quality grade. In nearly all samples, the fatty acid ethyl ester content was close to the threshold established for extra virgin olive oils indicating a non-excellent quality of the olive oils. Organoleptic evaluations, commonly called panel test, given by the nine labs were not consistent. Conclusions The EEC Regulation 2568/91 does not give any indication on the way to report the uncertainty of the results, and in the case of extra virgin olive oils with a borderline value, the way to report the fatty acid ethyl ester content, with or without the uncertainty, can create confusion in defining the olive oil quality grade. Panel test seemed to work well only in the case of extremely good olive oils, whereas, in commercial extra virgin olive oils with borderline value of fatty acid ethyl ester content, a different sensory sensibility seems to be in the different IOC labs. Graphical abstract Panel test and chemical analyses of commercial olive oils: a comparative study.

Abstract Low-field 1H NMR relaxometry is an important tool used to investigate on the most abundant components of intact foodstuffs based on relaxation parameters and amplitude of the NMR signals. In particular, information on water compartments, diffusion and movement can be obtained by detecting proton signals prevalently ascribable to H2O contained in foodstuffs. The main advantage of this technique is that it does not require any pretreatment of the sample and once developed, standard protocols based on rapid measurements can be easily transferred to quality control applications. An actual breakthrough for the low-field NMR application to food science has certainly been the development of unilateral NMR sensors. These devices present an attractive option for non-invasive assessment of compositional and microstructure of food materials. They are portable and allow easy sample access, which makes them attractive for quality control in industrial environments and directly on sealed packaged foods. A price to pay is the inhomogeneity of the magnetic field, which compromises the sensitivity of these devices. However, recent developments in unilateral magnets design offer larger sensitive volume, higher sensitivity and shorter dead times. In this brief review, we highlight the different uses of unilateral NMR devices in food analysis. Graphical abstract .

Actinidia deliciosa cv. Hayward fruit is renowned for its micro- and macronutrients, which vary in their levels during berry physiological development and postharvest processing. In this context, we have recently described metabolic pathways/molecular effectors in fruit outer endocarp characterizing the different stages of berry physiological maturation. Here, we report on the kiwifruit postharvest phase through an integrated approach consisting of pomological analysis combined with NMR/LC-UV/ESI-IT-MSn- and 2D-DIGE/nanoLC-ESI-LIT-MS/MS-based proteometabolomic measurements. Kiwifruit samples stored under conventional, cold-based postharvest conditions not involving the use of dedicated chemicals were sampled at four stages (from fruit harvest to pre-commercialization) and analyzed in comparison for pomological features, and outer endocarp metabolite and protein content. About 42 metabolites were quantified, together with corresponding proteomic changes. Proteomics showed that proteins associated with disease/defense, energy, protein destination/storage, cell structure and metabolism functions were affected at precise fruit postharvest times, providing a justification to corresponding pomological/metabolite content characteristics. Bioinformatic analysis of variably represented proteins revealed a central network of interacting species, modulating metabolite level variations during postharvest fruit storage. Kiwifruit allergens were also quantified, demonstrating in some cases their highest levels at the fruit pre-commercialization stage. By lining up kiwifruit postharvest processing to a proteometabolomic depiction, this study integrates previous observations on metabolite and protein content in postharvest berries treated with specific chemical additives, and provides a reference framework for further studies on the optimization of fruit storage before its commercialization.

The chemical profile of the female inflorescence extracts from seven Cannabis sativa L. dioecious cultivars (Carmagnola, Fibranova, Eletta Campana, Antal, Tiborszallasi, Kompolti, and Tisza) was monitored at three harvesting stages (4, 14, and 30 September), reaching from the beginning of flowering to end of flowering/beginning of seed formation, using untargeted nuclear magnetic resonance (NMR) and targeted (ultra-high-performance liquid chromatography (UHPLC) and spectrophotometry) analyses. The tetrahydrocannabinol content was always below the legal limits (Cannabis sativa L. inflorescences of each analyzed dioecious hemp cultivar presented a peculiar chemical profile affected by the harvesting stage. This information could be useful for producers and industries to harvest inflorescences in the appropriate stage to obtain samples with a peculiar chemical profile suitable for proper applications.

The metabolite profile of ten traditional apple cultivars grown in the Piedmont region (Italy) was studied by means of nuclear magnetic resonance spectroscopy, identifying an overall number of 36 compounds. A more complete assignment of the proton nuclear magnetic resonance (1H NMR) resonances from hydroalcoholic and organic apple extracts with respect to literature data was reported, identifying fructose tautomeric forms, galacturonic acid, γ-aminobutyric acid (GABA), p-coumaroyl moiety, phosphatidylcholine, and digalactosyldiacylglycerol. The chemical profile of each apple cultivar was defined by thorough quantitative NMR analysis of four sugars (fructose, glucose, sucrose, and xylose), nine organic acids (acetic, citric, formic, citramalic, lactic, malic, quinic, and galacturonic acids), six amino acids (alanine, asparagine, aspartate, GABA, isoleucine, and valine), rhamnitol, p-coumaroyl derivative, phloretin/phloridzin and choline, as well as β-sitosterol, fatty acid chains, phosphatidylcholine, and digalactosyldiacylglycerol. Finally, the application of PCA analysis allowed us to highlight possible differences/similarities. The Magnana cultivar showed the highest content of sugars, GABA, valine, isoleucine, and alanine. The Runsé cultivar was characterized by high amounts of organic acids, whereas the Gamba Fina cultivar showed a high content of chlorogenic acid. A significant amount of quinic acid was detected in the Carla cultivar. The knowledge of apple chemical profiles can be useful for industries interested in specific compounds for obtaining ingredients of food supplements and functional foods and for promoting apple valorization and preservation.

Torpedino di Fondi (TF) is a hybrid tomato landrace developed in Sicily and recently introduced in the south Lazio area along with the classical San Marzano (SM) cultivar. The present study aimed at characterizing TF tomatoes at both pink and red ripening stages, and at comparing them with traditional SM tomatoes. A multidisciplinary approach consisting of morphological, chemical (FT-ICR MS, NMR, HPLC, and spectrophotometric methods), and biological (antioxidant and antifungal in vitro activity) analyses was applied. Morphological analysis confirmed the mini-San Marzano nature and the peculiar crunchy and solid consistency of TF fruits. Pink TF tomatoes displayed the highest content of hydrophilic antioxidants, like total polyphenols (0.192 mg/g), tannins (0.013 mg/g), flavonoids (0.204 mg/g), and chlorophylls a (0.344 mg/g) and b (0.161 mg/g), whereas red TF fruits were characterized by the highest levels of fructose (3000 mg/100 g), glucose (2000 mg/100 g), tryptophan (2.7 mg/100 g), phenylalanine (13 mg/100 g), alanine (25 mg/100 g), and total tri-unsaturated fatty acids (13% mol). Red SM fruits revealed the greatest content of lipophilic antioxidants, with 1234 mg/g of total carotenoids. In agreement with phenolics content, TF cultivar showed the greatest antioxidant activity. Lastly, red TF inhibited Candida species (albicans, glabrata and krusei) growth.

Nine commercial hemp seed oils from different countries were studied using a multimethodological approach to obtain information about their quality and chemical composition. Due to the lack of a specific regulation for hemp seed oils, quality parameters used in the case of olive oils (free acidity, peroxides number, spectrophotometer parameters) and anisidine number were measured and compared with those reported for extra virgin olive oil (EVOO). Free acidity and peroxides number showed a great variability, ranging from 0.4 to 17.24% and from 4.32 to 22.14 meqO2/kg, respectively, whereas the anisidine number ranged from 0.11 to 3.58. K232 value turned out to be generally below the limit reported for EVOO, whereas K270 and ΔK values were higher, with respect to EVOO limits, due to the high amount of tri-unsaturated fatty chains. Colorimetric analysis showed a peculiar curve trend that could represent the fingerprint of this product. Untargeted nuclear magnetic resonance methodology allowed to measure the amount of fatty chains, ω-6:ω-3 ratio, β-sitosterol, and aldehydes. The ω-6:ω-3 ratio turned out to be, in some cases, different from that reported on the bottle labels. Finally, lipoperoxidation assays were also carried out under different storage (light and temperature) and time exposure conditions, confirming that the exposure to direct light is the condition that interferes more with the product quality.

The chemical characterization of local Italian potato cultivars is reported to promote their preservation and use as high quality raw material in food industries. Twenty potato (Solanum tuberosum L.) cultivars from Piedmont and Liguria Italian regions were investigated using NMR (Nuclear Magnetic Resonance) and RP-HPLC-PDA-ESI-MSn (Reversed Phase High-Performance Liquid Chromatography with Photodiode Array Detector and Electrospray Ionization Mass Detector) methodologies. Water soluble and lipophilic metabolites were identified and quantified. With respect to literature data, a more complete 1H (protonic) spectral assignment of the aqueous potato extracts was reported, whereas the 1H NMR assignment of potato organic extracts was reported here for the first time. Phenolics resulted to be in high concentrations in the purple–blue colored Rouge des Flandres, Bergerac, Fleur Bleu, and Blue Star cultivars. Servane, Piatlina, and Malou showed the highest amount of galacturonic acid, a marker of pectin presence, whereas Jelly cultivar was characterized by high levels of monosaccharides. Roseval and Rubra Spes contained high levels of citric acid involved in the inhibition of the enzymatic browning in fresh-cut potato. High levels of the amino acids involved in the formation of pleasant-smell volatile compounds during potato cooking were detected in Rouge des Flandres, Blue Star, Bergerac, Roseval, and Ratte cultivars. These results suggest that each local cultivar is characterized by a proper chemical profile related to specific proprieties that can be useful to obtain high quality industrial products.

Foods, food ingredients, and their balanced consumption are recognized to have an important role in achieving or maintaining a state of wellbeing by acting as carriers of functional components and bioactive molecules. However, the potential contribution of foods to consumers’ health has so far only been partially exploited. The rapidly evolving scenario of the coronavirus disease 2019 (COVID-19) pandemic is stimulating profound reflection on the relationships between food and the etiological agent, the severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2). Here, the status of knowledge regarding food as a possible defense/co-therapeutic strategy against the SARS-CoV-2 coronavirus is considered through the discussion of two main current lines of research. One line of research relates to the role of micronutrients, food components, and diets in the strengthening of the immune system through clinical trials; formulations could be developed as immune system enhancers or as co-adjuvants in therapies. The other line of research relates to investigation of the chemical interactions that specific food compounds can have with host or virus targets so as to interfere with the viral infective cycle of SARS-CoV-2. This line requires, as a first step, an in silico evaluation to discover lead compounds, which may be further developed through drug-design studies, in vitro and in vivo tests, and, finally, clinical trials to obtain therapeutic molecules. All of these promising strategies promote the role of food in preventive/co-therapeutic strategies to tackle the COVID-19 pandemic.

The chemical composition of the inflorescences from four Cannabis sativa L. monoecious cultivars (Ferimon, Uso-31, Felina 32 and Fedora 17), recently introduced in the Lazio Region, was monitored over the season from June to September giving indications on their sensorial, pharmaceutical/nutraceutical proprieties. Both untargeted (NMR) and targeted (GC/MS, UHPLC, HPLC-PDA/FD and spectrophotometry) analyses were carried out to identify and quantify compounds of different classes (sugars, organic acids, amino acids, cannabinoids, terpenoids, phenols, tannins, flavonoids and biogenic amines). All cultivars in each harvesting period showed a THC content below the Italian legal limit, although in general THC content increased over the season. Citric acid, malic acid and glucose showed the highest content in the late flowering period, whereas the content of proline drastically decreased after June in all cultivars. Neophytadiene, nerolidol and chlorogenic acid were quantified only in Felina 32 cultivar, characterized also by a very high content of flavonoids, whereas alloaromadendrene and trans-cinnamic acid were detected only in Uso-31 cultivar. Naringenin and naringin were present only in Fedora 17 and Ferimon cultivars, respectively. Moreover, Ferimon had the highest concentration of biogenic amines, especially in July and August. Cadaverine was present in all cultivars but only in September. These results suggest that the chemical composition of Cannabis sativa L. inflorescences depends on the cultivar and on the harvesting period. Producers can use this information as a guide to obtain inflorescences with peculiar chemical characteristics according to the specific use.

Bamano, King Creole, Sugarland, and DulceMiel hybrid tomato cultivars have been recently introduced in the Lazio area (Central Italy) to expand and valorize the regional/national market. Tomatoes from these cultivars, together with tomatoes from the native Fiaschetta cultivar, were sampled at the proper ripening time for the fresh market and characterized to obtain and compare their metabolite profiles. The Bligh−Dyer extraction protocol was carried out, and the resulting organic and hydroalcoholic fractions were analyzed by high-field Nuclear Magnetic Resonance (NMR) spectroscopy. NMR data relative to quantified metabolites (sugars, amino acids, organic acids, sterols, and fatty acids) allowed to point out similarities and differences among cultivars. DulceMiel hybrid and Fiaschetta native cultivars showed some common aspects having the highest levels of the most abundant amino acids as well as comparable amounts of organic acids, amino acids, stigmasterol, and linoleic and linolenic acids. However, DulceMiel turned out to have higher levels of glucose, fructose, and galactose with respect to Fiaschetta, reflecting the particular taste of the DulceMiel product. King Creole, Bamano, and Sugarland hybrid cultivars were generally characterized by the lowest content of amino acids and organic acids. King Creole showed the highest content of malic acid, whereas Bamano was characterized by the highest levels of glucose and fructose.

Over the last decade, the number of scientific publications in the metabolomics area has increased exponentially. The literature includes ~29,000 contributions (articles and reviews) during the period of 2009−2019, revealing metabolomics applications in a wide range of fields, including medical, plant, animal, and food sciences (this bibliographic data were retrieved from the SCOPUS database, searching “metabolomics” in keywords). The high applicability of this approach is due to its ability to qualitatively and quantitatively characterize the chemical profile of all the low molecular weight metabolites (metabolome) present in cells, tissues, organs, and biological fluids as end products of the cellular regulatory pathways. Thus, providing a snapshot of the phenotype of a biological system, metabolomics offers useful contributions to a comprehensive insight into the functional status of human, animal, plant, and microbe organisms. The contributions collected in this Special Issue (12 articles, one review and one technical report) report on the recent technical advances and practical applications of NMR spectroscopy to metabolomics analyses.

Metabolic profile of fresh turkey spermatozoa at three different reproductive period ages, namely 32, 44 and 56 weeks, was monitored by Nuclear Magnetic Resonance (NMR) spectroscopy and correlated to sperm quality parameters. The age-related decrease in sperm quality as indicated by reduction of sperm concentration, sperm mobility and osmotic tolerance was associated to variation in the level of specific water-soluble and liposoluble metabolites. In particular, the highest levels of isoleucine, phenylalanine, leucine, tyrosine and valine were found at 32 weeks of age, whereas aspartate, lactate, creatine, carnitine, acetylcarnitine levels increased during the ageing. Lipid composition also changed during the ageing: diunsaturated fatty acids level increased from 32 to 56 weeks of age, whereas a reduction of polyunsaturated fatty acids content was observed at 56 weeks. The untargeted approach attempts to give a wider picture of metabolic changes occurring in ageing suggesting that the reduction of sperm quality could be due to a progressive deficiency in mitochondrial energy producing systems, as also prompted by the negative correlation found between sperm mobility and the increase in certain mitochondrial metabolites.

In this review, fundamental aspects of the untargeted NMR-based methodology applied to fruit characterization are described. The strategy to perform the structure elucidation of fruit metabolites is discussed with some examples of spectral assignments by 2D experiments. Primary ubiquitous metabolites as well as secondary species-specific metabolites, identified in different fruits using an untargeted 1H-NMR approach, are summarized in a comprehensive way. Crucial aspects regarding the quantitative elaboration of spectral data are also discussed. The usefulness of the NMR-based metabolic profiling was highlighted using some results regarding quality, adulteration, varieties and geographical origin of fruits and fruit-derived products such as juices.

An NMR analytical protocol is proposed to characterize saffron samples of different geographical origin (Greece, Spain, Hungary, Turkey and Italy). A microwave-assisted extraction procedure was developed to obtain a comparable recovery of metabolites with respect to the ISO specifications, reducing the solvent volume and the extraction time needed. Metabolite profiles of geographically different saffron extracts were compared showing significant differences in the content of some metabolites.

A pilot study was carried out on five obese/overweight patients suffering from metabolic syndrome, with the aim to evaluate postprandial effects of high fat/high glycemic load meals enriched by blueberries. Postprandial urine samples were analyzed by 1H-NMR spectroscopy after 2 and 4 h from ingestion to identify potential markers of blueberry intake. Significant decrease of methylamines, acetoacetate, acetone and succinate, known indicators of type 2 diabetes mellitus, were observed after the intake of meals enriched with blueberries. On the other hand, an accumulation of p-hydroxyphenyl-acetic acid and 3-(3’-hydroxyphenyl)-3-hydropropionic acid originating from gut microbial dehydrogenation of proanthocyanidins and procyanidins was detected. Real-time PCR-analysis of mRNAs obtained from mononuclear blood cells showed significant changes in cytokine gene expression levels after meals integrated with blueberries. In particular, the mRNAs expression of interleukin-6 (IL-6) and Transforming Growth Factor-β (TGF-β), pro and anti-inflammation cytokines, respectively, significantly decreased and increased after blueberry supplementation, indicating a positive impact of blueberry ingestion in the reduction of risk of inflammation. The combined analysis of the urine metabolome and clinical markers represents a promising approach in monitoring the metabolic impact of blueberries in persons with metabolic syndrome.

Extra-virgin olive oil (383 samples; EVOOs) of three consecutive harvesting years from nine Italian regions were collected and submitted to an 1H NMR-chemometric protocol to characterize the samples according to their origin (geographical area and variety). A more complete assignment of the olive oil 1H spectrum in CDCl3 and DMSOd6 was reported identifying 24-methylencycolartanol. A single classification model provided the discrimination of EVOOs among the three geographical macro-areas (North, Islands, Center-South), whereas a hierarchical approach based on breaking the overall classification problem into a series of smaller linear discriminant analysis (LDA) sub-models was tested to differentiate olive oils according to their geographical regions. Specific compounds responsible for olive oil characterization were identified.

Due to renewed interest in the cultivation and production of Italian Cannabis sativa L., we proposed a multi-methodological approach to explore chemically and biologically both the essential oil and the aromatic water of this plant. We reported the chemical composition in terms of cannabinoid content, volatile component, phenolic and flavonoid pattern, and color characteristics. Then, we demonstrated the ethnopharmacological relevance of this plant cultivated in Italy as a source of antioxidant compounds toward a large panel of enzymes (pancreatic lipase, α-amylase, α-glucosidase, and cholinesterases) and selected clinically relevant, multidrug-sensible, and multidrug-resistant microbial strains (Staphylococcus aureus, Helicobacter pylori, Candida, and Malassezia spp.), evaluating the cytotoxic effects against normal and malignant cell lines. Preliminary in vivo cytotoxicity was also performed on Galleria mellonella larvae. The results corroborate the use of this natural product as a rich source of important biologically active molecules with particular emphasis on the role exerted by naringenin, one of the most important secondary metabolites.

An analytical approach including Panel Test, Isotope Ratio Mass Spectrometry (IRMS) and Nuclear Magnetic Resonance (NMR) spectroscopy was proposed to characterize Italian “Colline Pontine” PDO olive oils (40 samples) of two consecutive crop years. Our approach has evidenced the high quality of these olive oils. Only 6 of 40 olive oils samples were defined as “defective” by the official Panel Test due to the detection of negative sensory attributes. The low variability of isotopic data monitored by IRMS confirmed that the olive oil samples all came from a limited geographical area. NMR spectra did not evidence any chemical composition anomaly in the investigated samples. In order to assess the influence of harvesting year over the olive oil chemical composition, the NMR analysis was extended to other 22 olive oil samples of a third harvesting year. NMR data were submitted to two different statistical methods, namely, analysis of variance (ANOVA) and principal component analysis (PCA) allowing olive oils of three consecutive harvesting years to be grouped.

In this paper we report a comparative characterization of Small UnilamellarVesicles (SUVs), Large Unilamellar Vesicles (LUVs) and Multilamellar Vesicles (MLVs)prepared from 1-palmitoyl-2-oleoyl-sn-glycero-3-phospatidylcholine (POPC), carried outusing two NMR techniques, namely High Resolution NMR in solution and HighResolution–Magic Angle Spinning (HR-MAS). The size and size distributions of thesevesicles were investigated using the dynamic light scattering technique. An improvedassignment of the 1H-NMR spectrum of MLVs is also reported.

Nuclear magnetic resonance (NMR) is a powerful technique able to give us a relevant contribution in food analysis. In this review, some practical aspects of this technique (sample preparation, acquisition time, relaxation delay, etc) as well as some methods of spectral assignment of the spectra (2D and 1D selective technique) are reported. Some examples of NMR quantitative analyses are reported. In particular, the results relative to the NMR study of olive oils are discussed, among these: the comparison between conventional analyses and the NMR analysis in the olive oil characterization; the NMR determination of minor components such as squalene, cyclo-arthenol and chlorophyll in olive oil; the panel test and its relationship with NMR data; the geographical characterization of olive oils.

High-field Nuclear Magnetic Resonance (NMR) spectroscopy and Gas Chromatography (GC) were used to analyze 16 monovarietal olive oils obtained from few matched Mediterranean cultivars grown in experimental fields located in Italy and in the Catamarca region of Argentina. The Catamarca region is characterized by extreme pedoclimatic conditions and by a wild spontaneous vegetation. The proposed sampling allows to study the effect of different pedoclimatic conditions on olive oil composition. GC gives the fatty acid profile of olive oil samples. 1H and 13C NMR techniques provide different information: the 1H NMR spectrum allows the measurement of minor components of olive oils such as b-sytosterol, hexanal, trans-2-hexenal, formaldehyde, squalene, cycloartenol and linolenic acid; the 1C NMR spectrum allows to obtain information about glycerol tri-esters of olive oils, i.e., about their acyl composition and positional distribution on glycerol moiety. All the NMR and GC results have been submitted to Linear Discriminant Analysis (LDA) and Tree Cluster Analysis (TCA). A careful analysis of the statistical results allows to select the Mediterranean cultivars less affected by the climatic conditions present in the Catamarca region. The selected cultivars produce olive oils which keep their Mediterranean characteristics and which can be proposed as colonizing plants in this wild Argentine region.

Highly stable natural scaffolds which tolerate multiple amino acid substitutions represent the ideal starting point for the application of rational redesign strategies to develop new catalysts of potential biomedical and biotechnological interest. The knottins family of disulphide-constrained peptides display the desired characteristics, being highly stable and characterized by hypervariability of the inter-cysteine loops. The potential of knottins as scaffolds for the design of novel copper-based biocatalysts has been tested by engineering a metal binding site on two different variants of an ω-conotoxin, a neurotoxic peptide belonging to the knottins family. The binding site has been designed by computational modelling and the redesigned peptides have been synthesized and characterized by optical, fluorescence, electron spin resonance and nuclear magnetic resonance spectroscopy. The novel peptides, named Cupricyclin-1 and -2, bind one Cu(2+) ion per molecule with nanomolar affinity. Cupricyclins display redox activity and catalyze the dismutation of superoxide anions with an activity comparable to that of non-peptidic superoxide dismutase mimics. We thus propose knottins as a novel scaffold for the design of catalytically-active mini metalloproteins.