Search

The main objective of this review is to summarize the compositional characteristics and the health and functional properties of Mediterranean buffalo milk and whey derived from mozzarella cheese production. Several studies have investigated the composition of buffalo milk and in particular its fat, protein, and carbohydrates contents. These characteristics may change depending on the breed, feeding regime, and rearing system of the animals involved in the study, and also with the seasons. In particular, buffalo milk showed a higher nutritional value and higher levels of proteins, vitamins, and minerals when compared to milks produced by other animal species. Additionally, buffalo milk contains beneficial compounds such as gangliosides that can provide antioxidant protection and neuronal protection, and can improve bone, heart, and gastrointestinal health in humans.

In this work we report a lipidomics approach to study the effects of two diet systems on the composition of ovine milk. Milk from two groups of Sarda sheep grazing on 40% (P40) and 60% (P60) of pasture were analyzed by a UHPLC-QTOF-MS analytical platform and data submitted to multivariate statistical analysis. Pairwise partial least square discriminant analysis of the lipid profile of the data was carried out to classify samples and to find discriminant lipids. The two dietary groups were characterized by differences in triacylglycerols, phosphocholines and phosphatidylethanolamines levels. Discriminants of the P40 group were TG and PC containing in their backbone saturated medium chain FA thus suggesting greater de novo fatty synthesis in the mammary gland. On the other hand, the P60 group was characterized by TG and PC formed by unsaturated long chain FA originating from the diet or from lipid mobilization.

With an unsupervised GC–MS metabolomics approach, polar metabolite changes of the microalgae Coccomyxa melkonianii SCCA 048 grown under standard conditions for seven weeks were studied. C. melkonianii was sampled at the Rio Irvi River, in the mining site of Montevecchio-Ingurtosu (Sardinia, Italy), which is severely contaminated by heavy metals and shows high concentrations of sulfates. The partial-least-square (PLS) analysis of the GC–MS data indicated that growth of C. melkonianii was characterized by an increase of the levels of threonic acid, myo-inositol, malic acid, and fumaric acid. Furthermore, at the sixth week of exponential phase the lipid fingerprint of C. melkonianii was studied by LC-QTOF-MS. C. melkonianii lipid extract characterized through an iterative MS/MS analysis showed the following percent levels: 61.34 ± 0.60% for triacylglycerols (TAG); 11.55 ± 0.09% for diacylglyceryltrimethyl homoserines (DGTS), 11.34 ± 0.10% for sulfoquinovosyldiacylglycerols (SQDG) and, 5.29 ± 0.04% for lysodiacylglyceryltrimethyl homoserines (LDGTS). Noteworthy, we were able to annotate different fatty acid ester of hydroxyl fatty acid, such as FAHFA (18:1_20:3), FAHFA (18:2_20:4), FAHFA (18:0_20:2), and FAHFA (18:1_18:0), with relevant biological activity. These approaches can be useful to study the biochemistry of this extremophile algae in the view of its potential exploitation in the phycoremediation of polluted mining areas.

The aim of this work was to evaluate, by an untargeted metabolomics approach, changes of milk metabolites induced by the replacement of soybean hulls with cocoa husks in the ewes’ diet. Animals were fed with a soybean diet integrated with 50 or 100 g/d of cacao husks. Milk samples were analyzed by an ultra high performance liquid chromatograph coupled to a time of flight mass spectrometer (UHPLC-QTOF-MS) platform. Multivariate statistical analysis showed that the time of sampling profoundly affected metabolite levels, while differences between treatments were evident at the fourth week of sampling. Cocoa husks seem to induce level changes of milk metabolites implicated in the thyroid hormone metabolism and ubiquinol-10 biosynthesis.

This study aimed to evaluate the effects of different feedings on main traits and polar and semi-polar metabolite profiles of ovine milk. The milk metabolome of two groups of Sarda sheep kept under different grazing systems were analyzed by gas chromatography coupled with mass spectrometry (GC-MS) and multivariate statistical analysis (MVA). The results of discriminant analysis indicated that the two groups showed a different metabolite profile, i.e., milk samples of sheep kept under Grazing System 1 (GS1) were richer in nucleosides, inositols, hippuric acid, and organic acids, while milk of sheep under Grazing System 2 (GS2) showed higher levels of phosphate. Statistical analysis of milk main traits indicates that fat content was significantly higher in GS1 samples while milk from GS2 sheep had more urea, trans-vaccenic acid, and rumenic acid. MVA studies of the associations between milk main traits and metabolite profile indicated that the latter reflects primarily the long chain fatty acid content, the somatic cell count (SCC), and lactose levels. All together, these results demonstrated that an integrated holistic approach could be applied to deepen knowledge about the effects of feeding on sheep’s milk composition.

In this study, the polar metabolite profile of commercial yoghurt samples produced in Sardinia (Italy) from milk of local sheep and goats was studied by GC-MS and multivariate statistical data analysis (MVA). Milks underwent the same manufacturing procedures and yoghurts were analysed one day post-manufacture. Results of discriminant analysis indicated that the two yoghurt types had very different metabolite profiles, with different levels of health promoting compounds. Goats' milk yoghurt was richer in free amino acids, γ-aminobutyric acid, pyroglutamic acid and β-phenyllactic acid when compared with yoghurt produced with sheep's milk. Sheep's milk yoghurt was characterised by higher levels of myo-inositol, N-acetylgalactosamine and N-acetylglucosamine. Comparing yoghurt metabolites with those of the original milk, it was found that goats' milk underwent stronger metabolite changes after inoculum. The comparison between the two yoghurt types gave us a deeper insight on the effects of manufacture on different milks.

Nuclear magnetic resonance (NMR) spectroscopy, which is one of the most powerful “omics” analytical platforms, has been broadly adopted recently in foodomics. 1H NMR has been applied to the study of the metabolite profile of dairy products throughout the supply chain, in relation to different aspects such as animal health, milk quality, geographical origin and cheese ripening process. This review reports and discusses the literature on the topic, also collecting the identified metabolites in a descriptive table and depicting them in a Venn diagram for both milk and cheese; moreover, experimental details of the reviewed papers have been reported. The present review provides an exhaustive state-of-the-art in the field of dairy products, addressing both NMR experts and non-experts to the still unexplored potential applications of NMR in dairy characterisation, and in general in foodomics.

Fossa cheese is a typical Italian cheese characterised by ripening in pits dug in tuffaceous rock. In this work, 1H NMR spectroscopy was applied to characterise the lipid fraction and the metabolite profile of Fossa cheese produced with sheep's milk. Samples were collected before and after ripening in different pit environments. The higher levels of free amino acids (FAAs) found in samples suggest that cheeses underwent a strong proteolytic process. Differences in quantity and variety of FAAs were influenced by the two ripening environments. Diacylglycerols and butyric acid, which can be linked to lipolysis, were detected in all the samples. Longer ripened samples had higher contents of rumenic acid (18:2 cis-9, trans-11) and glycerol, and lower contents of lactate and citrate. The presence of tyramine was observed by two-dimensional NMR, while cadaverine was not detected in the samples.

Cardiac arrest (CA) is not a uniform condition and its pathophysiology strongly depends on its cause. In this work we have used a metabolomics approach to study the dynamic metabolic changes occurring in the plasma samples of a swine model following two different causes of CA, namely asphyxia (ACA) and ventricular fibrillation (VFCA). Plasma samples were collected at baseline and every minute during the experimental phases. In order to identify the metabolomics profiles characterizing the two pathological entities, all samples were analysed by 1H NMR spectroscopy and LC-MS/MS spectrometry.The metabolomics fingerprints of ACA and VFCA significantly differed during the peri-arrest period and the resuscitation phase. Major alterations were observed in plasma concentrations of metabolites related to tricarboxylic acid (TCA) cycle, urea cycle, and anaplerotic replenishing of TCA. ACA animals showed significant metabolic disturbances during the asphyxial and CA phases, while for VFCA animals this phenomenon resulted shifted at the resuscitation phase. Interestingly, starting from the asphyxial phase, the ACA animals were stratified in two groups based on their metabolomics profiles that resulted to be correlated with the clinical outcome. Succinate overproduction was observed in the animals with the worse outcome, suggesting a potential prognostic role for this metabolite.

Ovine milk (Sarda breed) with high somatic cell count (SCC) (>1 × 106 cell mL−1) was compared with similar milk of low SCC (

Black truffle is characterized by a black ascocarp and white veins. This hypogeous fruit body is known for its aroma. Understanding metabolic variation during ripening can shed light on truffle biology. In this work, the comprehensive polar metabolome and the volatile organic compounds of T. melanosporum were studied at different ripening stages by means of a metabolomic approach using GC–MS. Multivariate statistical data analysis indicated that the metabolic profile changed during ripening and that the metabolites that mostly discriminated truffles in the early ripening stages belonged to the classes of carbohydrates, while free fatty acids and amino acids, among which precursors of VOCs, characterized the late stages of ripening. Principal component analysis of the volatilome indicated that dimethylsulfide and dimethyldisulfide characterized most of the samples collected in December-January, while 1-octen-3-ol samples collected in February-March.

Infrared spectroscopy is widely applied in the wine sector. The medium infrared (MIR) spectral region between 1800 and 900 cm-1 is very informative for polyphenols. Aim of this work was to perform an in-depth analysis of this spectral region of polyphenolic wine extracts. To this goal evolution of the polyphenolic fractions of white (Vermentino) and red (Cannonau) typical Sardinian wines was studied during wine-making. Wine polyphenolic extracts, obtained by solid phase extraction, were analyzed by Attenuated Total Reflectance-Fourier Transform Infrared (ATR-FTIR) and UV–Vis spectroscopy. Spectral data from the two techniques were integrated and results depicted as Heat Map of the correlation coefficient values allowing a more accurate characterization of the MIR fingerprint region. For Cannonau, correlations between absorptions in the 420–650 and 380 nm visible spectral ranges allowed assignment of MIR peaks to anthocyanins (1016 and 1198 cm-1) and flavonols (1159 and 1277 cm-1), respectively. In Vermentino we identified MIR bands due to non-flavonols and others arising from flavonols (1376 and 1407 cm-1), present in this white wine where vinification allows short time contact with grape skins. During time, intensities of MIR bands at lower frequencies assigned to the sugar moiety of glycosylated phenols decreased in both wines.

Donkey milk is considered a potential substitute to human milk for infants affected by cows’ milk protein allergy. With the aim to widen our knowledge on this valuable food, we explored the compositional characteristics of Sardinian donkey milk. Donkey milk showed a low lipid content and high lysozyme levels compared to human milk, and a bacterial count below the recommended threshold. Hydrophilic compounds such as amino acids, organic acids and mono and disaccharides, were analyzed by GC-MS for donkey milk, formula milk and human milk. Results of the multivariate statistical analysis indicated that the metabolite profile of donkey milk is more similar to human milk than cow milk based formulae, the latter being richer in sugars and lower in amino acids. Moreover, modifications of human milk and donkey milk metabolite profiles during lactation time were studied. An increase of protein levels was observed in donkey milk, while in human milk pyroglutamic acid and myo-inositol levels increased and decreased, respectively.

Thermization is a sub-pasteurization heat treatment of cheese milk (at 57-68°C for 15-30 s) aimed to reduce the number of undesirable microbial contaminants with reduced heat damage to the indigenous milk enzymes. In this work, the effects of milk thermization on the compositional parameters, proteolysis indices, free fatty acid levels, and low molecular weight metabolite profiles of ovine cheese were studied. Cheese samples at different ripening stages and produced in 2 different periods of the year were analyzed. While the effects of milk thermization on cheese macro-compositional parameters and free fatty acid levels were not evident due to the predominant effects of milk seasonality and cheese ripening stage, the gas chromatography-mass spectrometry based metabolomics approach of ovine cheese produced from raw and thermized milk highlighted strong differences at the metabolite level. Discriminant analysis applied to gas chromatography-mass spectrometry data provided an excellent classification model where cheese samples were correctly classified as produced from raw or thermized milk. The metabolites that mostly changed due to the thermization process belonged to the classes of free amino acids and saccharides. Gas chromatography-mass spectrometry-based metabolomics has proven to be a valid tool to study the effect of mild heat treatments on the polar metabolite profile in ovine cheese.

Despite the worldwide consumption of bovine milk, dairy products from small ruminants, such as goat's and sheep's milk, are gaining a large interest especially in the Mediterranean area. The aim of this work was to study the metabolite profiles of 30 sheep's and 28 goat's milk using an untargeted metabolomics approach by a gas chromatography coupled with mass spectrometry (GC-MS) analysis. Results showed several differences in the metabolite profiles: arabitol, citric acid, α-ketoglutaric acid, glyceric acid, myo-inositol, and glycine were more abundant in sheep's milk, while goat's milk had higher levels of mannose-6-phosphate, isomaltulose, valine, pyroglutamic acid, leucine, and fucose. Associations between metabolite profile and milk compositional traits were also found. Predictive capabilities of statistical models indicated a good correlation between the metabolite profile and the protein content in sheep's milk, and with the fat content in goat's milk. This work leads to a better understanding of milk metabolites in small ruminants and their role in the evaluation of milk properties.

Italian buffalo mozzarella (BM) cheese metabolite profile and microbial communities were characterised and compared to cow mozzarella (CM). Polar metabolite profiles were studied by gas-chromatography mass-spectrometry (GC-MS) and results elaborated by multivariate analysis (MVA). BM produced using natural whey starter cultures (NWS) exhibited a higher microbial diversity with less psychrotrophic bacteria. BM samples were higher in threonine, serine, valine, and lower in orotic acid and urea. CM produced with commercial starters (CMS) had the highest count of Streptococcus thermophilus and higher levels of galactose and phenylalanine. CM obtained by direct acidification (CMA) had lower microbial counts and higher levels of urea and sugars. Orotic acid was the only metabolite linked to milk animal origin. Results indicated that this metabolite pool well reflects the different production protocols and microbial complexity of these dairy products. This approach can help to protect the designation of origin of Italian buffalo mozzarella.

The effect of a diet enriched with mullet bottarga on the lipid profile (total lipids, total cholesterol, unsaturated fatty acids, α-tocopherol, and hydroperoxides) of plasma, liver, kidney, brain, and perirenal adipose tissues of healthy rats was investigated. Rats fed a 10% bottarga enriched-diet for 5 days showed body weights and tissue total lipid and cholesterol levels similar to those of animals fed control diet. Univariate and multivariate results showed that bottarga enriched-diet modified the fatty acid profile in all tissues, except brain. Significant increases of n-3 PUFA, particularly EPA, were observed together with a 20:4 n-6 decrease in plasma, liver, and kidney. Perirenal adipose tissue showed a fat accumulation that reflected the diet composition. The overall data suggest that mullet bottarga may be considered as a natural bioavailable source of n-3 PUFA and qualify it as a traditional food product with functional properties and a potential functional ingredient for preparation of n-3 PUFA enriched foods.

In this study the antioxidant activity of methanol extracts obtained from Mediterranean fruit products (prickly pear fruit jam and cream, myrtle berries jam, orange and mandarin-orange marmalades) was evaluated and compared in several in vitro models of oxidative stress. The compositional profile of methanol extracts (carbohydrates, organic acids, amino acids, and main phenolic compounds) was characterized by 1 H NMR spectroscopy and the total phenol content was estimated by the Folin–Ciocalteu procedure. All extracts showed protective effect against thermal-cholesterol degradation, strictly correlated to total phenols. Extracts from prickly pear cream and myrtle berries jam preserved liposomes from Cu 2 + -induced oxidation, inhibiting the reduction of polyunsaturated fatty acids and the increase of malondialdehyde. Extracts from prickly pear cream and citrus marmalades significantly reduced the reactive oxygen species generation induced by tert -butylhydroperoxide in Caco-2 cell culture. The results of this work qualify all tested Mediterranean fruit preserves as a good source of biologically active components with considerable antioxidant potential.

While neurochemical metabolite modifications, determined by different techniques, have been diffusely reported in human and mice brains affected by transmissible spongiform encephalopathies (TSEs), this aspect has been little studied in the natural animal hosts with the same pathological conditions so far. Herein, we investigated, by high resolution (1)H NMR spectroscopy and multivariate statistical data analysis, the brain metabolite profile of sheep exposed to a scrapie agent in a naturally affected flock. On the basis of clinical examinations and western blotting analysis for the pathological prion protein (PrP(Sc)) in brain tissues, sheep were catalogued as not infected (H), infected with clinical signs (S), and infected without clinical signs (A). By discriminant analysis of spectral data, comparing S vs. H, we found a different metabolite distribution, with inosine, cytosine, creatine, and lactate being higher in S than in H brains, while the branched chain amino acids (leucine, isoleucine, and valine), phenylalanine, uracil, tyrosine, gamma-amino butyric acid, total aspartate (aspartate + N-acetyl aspartate) being lower in S. By a soft independent modelling of class analogy approach, 1 out of 3 A samples was assigned to class H. Furthermore, A brains were found to be higher in choline and choline-containing compounds. By means of partial least squares regression, an excellent correlation was found between the PrP(Sc) amount and the (1)H NMR metabolite profile of infected (S and A) sheep, and the metabolite mostly correlated with PrP(Sc) was alanine. The overall results, obtained using different chemometric tools, were able to describe a brain metabolite profile of infected sheep with and without clinical signs, compared to healthy ones, and indicated alanine as a biomarker for PrP(Sc) amounts in scrapie brains.

1H NMR spectroscopy was used to investigate changes in the low molecular weight metabolic profile of raw mullet (Mugil spp.) roes during frozen storage and upon processing. NMR data were analysed by Principal Component Analyses (PCA). In the model constructed using frozen roes, no statistical significant metabolic modifications were observed in the first six months of storage, while choline derivatives, dimethylamine, lactate, and most of the free amino acids were identified as changing with statistical significance (p

The aim of this work was to evaluate the impact of the addition of two lactic acid bacteria (LAB) strains, namely Lactobacillus casei-VC199 and Enterococcus lactis-BT161, on the composition of goat cheese at 30 and 60 d of ripening. In the metabolite and lipid profiles, as determined by 1H NMR spectroscopy, we found the primary products of lipolysis: free fatty acids (FFA) and diacylglycerols; of glycolysis: organic acids; and of proteolysis: free amino acids (FAA). The cheese volatilome, monitored over the ripening period by SPME-CG-MS, indicates the mechanism by which these primary metabolic products are converted to flavor compounds. Principal Component Analysis (PCA) suggests that the two LAB strains differently affect the metabolite and volatile compound content of the cheeses, the difference being the greatest at 60 d of cheese ripening. Cheese produced with Lb. casei had greater quantities of FAA, FFA, and organic acids than E. lactis cheese. The volatilome of samples inoculated with E. lactis was characterized by higher ketone content, while Lb. casei produced more acids and esters. The results of this work highlight the potential and complementarity of NMR and SPME-GC-MS analytical techniques to investigate the impact of LAB on cheese compositional characteristics.

Seeds of Citrus plants (Rutaceae), an major agro‐industrial waste, are a potential source of valuable by‐products. The chemical composition, the antioxidant profile, and the biological/nutritional properties of fixed oils (SFE oils) obtained by supercritical CO₂ extraction (at 300 bar and 40 °C) from seeds of mandarin (Citrus reticulata), lemon (Citrus limon), and grapefruit (Citrus paradisi), discarded by a local agro‐alimentary industry are studied. The yields and compositions of SFE oils are compared to oils obtained by n‐hexane extraction of Citrus seeds in a Soxhlet apparatus (SoxE oils). Linoleic (35–42%), oleic (22–28%), palmitic (21–25%), α‐linolenic (4–10%), and stearic (4–7%) are the main oil fatty acids, while monolinolein and dilinolein derivatives represent the main triacylglycerols in SFE oils, determined by GC‐FID and HPLC‐DAD/ELSD techniques. Citrus SFE oils show lower yields than SoxE oils but similar chemical profiles. Principal components analysis applied to fatty acid and triacylglycerol data indicates that the oils from different seeds are tightly clustered. Moreover, SFE oils show radical scavenging activities (ABTS assays), an inhibitory effect on the growth of murine B16F10 melanoma cells and on the mushroom tyrosinase activity. Citrus SFE oils and de‐coated seeds are also evaluated for their attractant effect on the Mediterranean fruit fly Ceratitis capitata by behavioral assays. The results qualify Citrus SFE oils as a potential natural, environmentally‐friendly, resource for food/pharmaceutical applications. Practical Applications: The environmentally‐friendly supercritical CO₂ extraction of waste lemon, mandarin, and grapefruit seeds gives edible fixed oils a richness in essential fatty acids, suitable for human nutrition and the preparation of nutraceuticals and pharmaceuticals. Edible fixed oils obtained from lemon, mandarin, and grapefruit seeds by SFE‐CO₂ extraction show high levels of essential fatty acids, antioxidant, anticancer, and antityrosinase activity.

In this feasibility study, we propose, for the first time, (1)H NMR spectroscopy coupled with mathematical strategies as a valid tool for body fluid (BF) trace identification in forensic science. In order to assess the ability of this approach to identify traces composed either by a single or by two different BFs, samples of blood, urine, saliva, and semen were collected from different donors, and binary mixtures were prepared. (1)H NMR analyses were carried out for all samples. Spectral data of the whole set were firstly submitted to unsupervised principal component analysis (PCA); it showed that samples of the same BF cluster well on the basis of their characterizing molecular components and that mixtures exhibit intermediate characteristics among BF typologies. Furthermore, samples were divided into a training set and a test set. An average NMR spectral profile for each typology of BF was obtained from the training set and validated as representative of each BF class. Finally, a fitting procedure, based on a system of linear equations with the four obtained average spectral profiles, was applied to the test set and the mixture samples; it showed that BFs can be unambiguously identified, even as components of a mixture. The successful use of this mathematical procedure has the advantage, in forensics, of overcoming bias due to the analyst's personal judgment. We therefore propose this combined approach as a valid, fast, and non-destructive tool for addressing the challenges in the identification of composite traces in forensics.

The salted and dried product of tuna roe (bottarga) is a seafood characteristic of the Mediterranean area and exported all over the world. Samples of bottarga from bluefin tunas (Thunnus thynnus, L.) caught in the southwest Mediterranean sea were analysed. The samples were characterised by high content of marine wax esters (55-67 mol% of lipid classes), of docosahexaenoic (22:6 n-3, 25 w%) and oleic (18:1 n-9, 19 w%) fatty acids. Cholesterol was detected as 7-9 w% of lipids. Free fatty acids, index of lipid hydrolysis, represented 32-39 mol% over total fatty acids. Among metabolites, nutrients as taurine, nicotinamide and β-alanine, were found. The microflora comprised staphylococci, enterococci (2.2 log(10)CFU/g) and lactic acid bacteria (3 log(10) CFU/g). The food-borne pathogens Staphylococcus aureus, Listeria monocytogenes and Salmonella spp. were not detected. These findings indicate tuna bottarga as valuable source of nutrients.

Nowadays metabolomics is a widely accepted approach in several scientific disciplines, especially in food science. The possibility to identify a wide range of metabolites (untargeted analysis) allowed to evaluate various food characteristics, regarding quality, adulteration, geographical origin, as well as secondary species-specific metabolites endowed with nutraceutical properties. In the present chapter, latest findings of plant-based foods investigated by NMR-based metabolomics are presented. Almost all of the recent studies were focused on quality assessment and authenticity; different aspects such as geographical origin, metabolic modifications upon stress, nutraceutical properties, and fraud detection are described as well. The here reported plant-based foods are balsamic and traditional balsamic vinegars, cereals, cocoa, coffee, fruits, legumes, spices, vegetables and vegetable oils, wine, beer, and spirits. A brief paragraph is concerning organic and conventional foods, which is a new growing scientific field of interest for researchers encouraged by the increasing consumers' demand. The results here reported testify the capability and the power of this approach thus endorsing NMR spectroscopy as a valid alternative or complement to the chemical and physical analysis nowadays routinely applied for the quality assessment.

Breast milk (BM) is the gold standard in neonatal nutrition. When BM is not available, it can be substituted or integrated with commercial infant formulas, sold under different brands and formulations. The low-molecular-weight hydrophilic compounds in various formula milk (FM) brands and BM samples were analyzed by GC-MS and multivariate statistical data analysis. Results highlighted that FM formulations, besides being strongly different from BM, are diverse especially in regard to the addition of oligosaccharides and other nutrients. Moreover, the 1H NMR spectra of the aqueous and of the lipid fractions of FM samples exhibited differences due to the diverse formulations. Strengths and weaknesses of the two analytical approaches will be discussed also in the light of the nutritional reports.

In the last years, researchers focused their studies in the development of high throughput omics technologies. Along with the main omics, namely genomics, transcriptomics, proteomics and metabolomics, a varieties of related subdisciplines (lipidomics, interactomics, epigenomics etc) raised to exploit several topics like food science, health and disease, nutrition etc. These techniques provide a wide vision of the metabolome, the entire biochemical complement present within every organism. The application of these broad vision to food science represents the comprehensive, high-throughput approach for the exploitation of food science in the light of an improvement of human nutrition and it is known under the name of Foodomics. This allowed researchers to approach the study of foods in their entire domain, following the evolution of all the components, as a consequence, for example, of the use of improved packaging materials, of new process to produce foods with added nutritional values, and modification of sensory characteristics upon food modification. In the present work, high resolution NMR is presented as a valid tool in metabolomics studies (1-3) to follow the metabolite profiles during the shelf life of foods.

Objectives: 1H NMR-metabolomic approach was used to investigate QTc interval correlation with plasma metabolic profiles in shiftworkers. Methods: Socio-demographic data, electrocardiographic QTc interval and plasma metabolic profiles from 32 male shiftworkers, were correlated by multivariate regression analysis. Results: We found a positive correlation between QTc interval values, body mass index, glycemia and lactate level and a negative correlation between QTc interval and both pyroglutamate and 3-hydroxybutyrate plasma level. Conclusions: Our analysis provides evidence of the association between clinical, metabolic profiles and QTc interval values. This could be used to identify markers of early effects and/or susceptibility in shiftworkers.

Cynomorium coccineum L. is a non-photosynthetic plant, spread over Mediterranean countries, amply used in traditional medicine. We investigated the composition and effect on intestinal Caco-2 cell viability and lipid profile of fixed oil obtained from dried stems of the plant. Oil isolation has been performed by supercritical fractioned extraction with CO2. 13C NMR spectroscopy has been used to study the molecular composition of oil lipids; fatty acid composition was identified using GC and HPLC techniques. The fixed oil was composed mainly by triacylglycerols and derivates. The main fatty acids were 18:1 n-9 (38%), 18:2 n-6 (20%), 16:0 (15%), and 18:3 n-3 (10.8%). The oil showed a significant in vitro inhibitory effect on the growth of colon cancer undifferentiated Caco-2 cells. Moreover, cell viability, lipid composition, and lipid peroxidation were measured in intestinal epithelial cells (differentiated Caco-2 cells) after 24 h incubation with fixed oil. The oil did not show a toxic effect on colon epithelial cell viability but induced a significant change in fatty acid composition, with a significant accumulation of the essential fatty acids 18:3 n-3 and 18:2 n-6. The results showed remarkable biological activity of Maltese mushroom oil, and qualify it as a potential resource for food/pharmaceutical applications.

In this work, we report the feasibility study to predict the properties of neat crude oil samples from 300-MHz NMR spectral data and partial least squares (PLS) regression models. The study was carried out on 64 crude oil samples obtained from 28 different extraction fields and aims at developing a rapid and reliable method for characterizing the crude oil in a fast and cost-effective way. The main properties generally employed for evaluating crudes' quality and behavior during refining were measured and used for calibration and testing of the PLS models. Among these, the UOP characterization factor K (KUOP) used to classify crude oils in terms of composition, density (D), total acidity number (TAN), sulfur content (S), and true boiling point (TBP) distillation yields were investigated. Test set validation with an independent set of data was used to evaluate model performance on the basis of standard error of prediction (SEP) statistics. Model performances are particularly good for KUOP factor, TAN, and TPB distillation yields, whose standard error of calibration and SEP values match the analytical method precision, while the results obtained for D and S are less accurate but still useful for predictions. Furthermore, a strategy that reduces spectral data preprocessing and sample preparation procedures has been adopted. The models developed with such an ample crude oil set demonstrate that this methodology can be applied with success to modern refining process requirements. Copyright © 2012 John Wiley & Sons, Ltd.

(1)H NMR spectroscopy was employed to study the modifications over time of the water-soluble low molecular weight metabolites extracted from samples of salted and dried mullet (Mugil cephalus) roes (mullet bottarga) stored at different conditions. Samples of grated mullet bottarga were stored for 7 months at -20 °C, at 3 °C, and at room temperature in the presence and in the absence of light and then timely extracted and analyzed by NMR. Principal component multivariate data analysis applied to the spectral data indicated that samples stored at -20 °C maintained similar features over time whereas, along PC1, samples stored at room temperature in the presence and in the absence of light showed, over time, marked metabolite modifications. The comparative analysis of the integrated areas of the selected regions of the (1)H NMR spectra indicated that the major compositional changes due to storage conditions were (i) the increase of the derivatives of the breakdown of phosphatidylcholine (choline, phosphorylcholine, and glycerol), (ii) the breakdown of nucleosides, (iii) the decrease of methionine, tryptophan, and tyrosine, and (iv) the cyclization of creatine. These changes were observed at different storage conditions, with more pronounced trends in the samples stored at room temperature. The role of metabolites in food aging is discussed.

Nuclear magnetic resonance (NMR) spectroscopy combined with multivariate data analysis (MVA) was used to investigate the molecular components of the aqueous extract of samples of bottarga, that is, salted and dried mullet (Mugil cephalus) roe, manufactured in Sardinia (Italy) from mullets of known and unknown geographical provenience. Principal component analysis (PCA) applied to the processed (1)H NMR spectra indicated that samples tend to cluster according to their geographical origin and also on the basis of storage and manufacturing procedures. The most important metabolites that characterized grouping of samples are the free amino acids methionine (Met), glutamate (Glu), histidine (His), phenylalanine (Phe), tyrosine (Tyr), and isoleucine (Ile); trimethylamine (TMA) and dimethylamine (DMA), both biomarkers of degradation; nucleotides and derivatives; choline (Cho) and phosphorylcholine (P-cho); and lactate (Lac).

In this work the molecular fatty components of Pecorino Sardo Protected Designation of Origin (PS PDO) cheese were characterized through an exhaustive investigation of the 1H- and 13C-NMR spectra of the extracted lipids. Several fatty acids (FA), such as long chain saturated, oleic, linoleic, linolenic, butyric, capric, caprylic, caproic, trans vaccenic, conjugated linoleic acid (cis9, trans11–18:2), and caproleic (9–10:1) were unambiguously detected. The positional isomery of some acyl groups in the glycerol backbone of triacylglycerols (TAG) was assessed. Furthermore, the NMR signals belonging to sn-1,2/2,3, sn-1,3 diacylglycerols (DAG), and free fatty acids (FFA) were analysed as a measure of lipolytic processes on cheese. Lastly, 1H-NMR resonances of saturated aldehydes and hydroperoxides were detected, their very low intensity indicating that the lipid oxidation process can be considered to be of minor relevance in Pecorino Sardo cheese.

Mullet bottarga is a food delicacy obtained by salting and drying the intact roes of mullet (Mugil spp.). The fatty acid and fatty alcohol compositions of different samples of bottarga were studied by means of gas chromatography (GC) and multivariate analysis (MVA). High percentages of beneficial n-3 PUFA, among which docosahexaenoic acid (DHA) (22:6n-3, 11.9%) and eicosapentaenoic acid (EPA) (20 : 5n -3, 8.6%), were detected. Differences in the concentrations of unsaturated FA and FAL were observed among samples, while saturated components showed little variations. On the other hand, the total contents of saturated, monounsaturated and polyunsaturated components were similar. The principal component analysis loadings bi-plot showed that n-6 PUFA concentrations were inversely correlated to those of n-3 PUFA, except for DHA that showed no correlations. Correlations between FAL concentrations were also observed. Furthermore, integrating our GC data with those from the literature on mullet and tuna bottarga, the MVA showed that both bottarga typologies exhibit a similar trend in the FA distribution and that 16:0 and 16:1 n-7 FA are the variables with the highest discriminant power. In this work, we demonstrated the usefulness of the application of MVA to GC data to extract meaningful information otherwise hidden in the amount of data.

The lipid composition and oxidative stability of mullet (Mugil cephalus) raw roes and cured products (bottarga) from two different fishing areas have been studied and compared to find lipid modifications due to manufacturing procedures. Moreover, n-3 PUFA oxidation in raw roes and cured products was monitored during storage at -20 °C, and in grated sample of bottarga at room temperature. Oxidative degradation of n-3 PUFA was evaluated by conjugated dienes fatty acids hydroperoxides determination. The treatments on mullet roe did not affect the lipid level (fatty alcohols and acids, cholesterol) and the amount of hydroperoxides. No significant difference is observed between n-3 PUFA levels during processing and at different storage conditions. The order of oxidative stability, as calculated by the hydroperoxides determination was: grated bottarga < whole bottarga < raw roe.

Samples of mullet (Mugil cephalus) roes from two different fishing areas were studied by means of 1 H, 13 C and 31 P NMR and GC techniques. The lipid fraction of unprocessed roes and that of the corresponding salted and dried commercial products "bottarga" were analyzed and the data compared. Roes of mullets from different origin showed different composition regarding mainly triacylglycerols, monounsaturated and n-3 polyunsaturated fatty acids. The NMR spectra of processed roes, compared to those of the corresponding raw materials, showed a release of free fatty acids and the formation of other minor molecular components, such as free fatty alcohols, lysophospholipids, and diacylglycerols, thus indicating that hydrolytic processes were the main consequence of manufacturing. An increase of cholesterol ester concentration after processing was also detected. Through the analysis of the 31 P NMR spectra, it was possible to follow the fate of the phospholipids and the formation of lysophospholipids induced by the salting and drying procedures.

Solid-state (13)C nuclear magnetic resonance (NMR) and elemental analysis techniques were used to monitor the degradation of wheat bran by the white-rot fungus Pleurotus ostreatus during a 62-day cultivation period. The weight loss and in vitro organic matter digestibility of the substrate were also evaluated after fungal treatment. The (13)C NMR spectra of degraded wheat bran samples showed a lower content in carbohydrates and a higher content in aliphatic and carboxylic groups than the untreated control sample. In parallel, changes in the wheat bran elemental composition evidenced a decrease in carbon content and a concomitant increase in nitrogen and oxygen content during mycelium growth. These results clearly indicate the occurrence of progressive changes in the composition of wheat bran during fungal treatment and are interpreted in terms of preferential degradation of amorphous vs. crystalline polysaccharides by the fungal mycelium and accumulation of proteins in the substrate. At the end of the cultivation period, the treated samples experienced an average weight loss of 20% and an increase in organic matter digestibility of 17%.