In this study, for the first time urinary NMR-based metabolomics was applied to investigate the physiological alterations associated with occupational exposure in ceramic manufacturing workers. Multivariate analysis revealed a distinctive metabolic signature with exposure, characterized by a depletion of both aliphatic and aromatic amino acids and a concomitant accumulation of branched-chain amino acid catabolites. Alterations in tricarboxylic acid (TCA) cycle intermediates, including citrate and succinate, suggest an involvement of mitochondrial energy metabolism, reflecting adaptive responses to oxidative stress and increased protein turnover. Notably, glycine levels were found increased, consistent with its central role in antioxidant defense and xenobiotic detoxification. Furthermore, changes in urinary host-microbiome co-metabolites, such as 4-hydroxyphenylacetate and phenylacetylglycine, indicate the potential modulation of gut microbial activity in response to occupational exposure. While limited by the small cohort, this study demonstrates the feasibility of NMR-based urinary metabolomics for the non-invasive biomonitoring of workers and suggests its potential as a useful tool for detecting subtle metabolic perturbations associated with complex occupational exposures.

Root exudates are crucial for driving belowground ecosystem dynamics and subterranean chemical interactions. Cyperus rotundus (purple nutsedge) is a highly invasive weed, notoriously resistant to conventional control and causing significant crop losses globally. Sorghum bicolor is well-known for producing allelopathic compounds via root exudates. The metabolic shifts occurring during the direct interaction between C. rotundus and allelopathic crop S. bicolor are yet unexplored. In this study, we established an in vitro protocol for the isolation of root exudates from solid growth medium and employed a non-targeted 1H-NMR spectroscopy approach to fingerprint the hydrophilic and lipophilic root exudates within an in vitro co-culture system. A total of 21 metabolites, including carbohydrates, phenolics, peptides and fatty acids were identified. Notably, three new sterols including (3β)-3-hydroxy-6-methylstigmast-20(22)-en-14-oic acid, 6-methylstigmast-20(22)-en-14-oic acid derivative 1 and 6-methylstigmast-20(22)-en-14-oic acid derivative 2 were univocally assigned. Comparative analysis revealed that co-cultivation induced specific metabolic changes rather than a general increase in exudation. Specifically, the cyanogenic glycoside dhurrin, a primary allelochemical in S. bicolor, significantly decreased in co-cultures, while phytoalexins B, detected in individual C. rotundus exudates, was absent in co-cultures. However, no significant reduction in root biomass was observed for either species over the 12-day experimental period. These findings suggest that while root-root proximity triggers specific secondary metabolites shifts, these changes did not translate into immediate growth inhibition under the tested conditions. This study provides the first non-targeted metabolic profiling of the direct belowground interaction between S. bicolor and C. rotundus and highlights the complexity of modulating allelopathic responses in sterile environments.

Saffron (Crocus sativus L.) is widely cultivated for the spice obtained from the stigmas, while the remaining floral biomass is discarded as biowaste. Accessing the phytochemical composition of these residues could enable their valorization as a low-cost and sustainable resource for nutraceutical applications. In this context, a quantitative H-1 NMR-based metabolite profiling approach, complemented by HPLC-DAD and LC-MS, was employed to comprehensively characterize saffron biowaste. A total of 40 metabolites were identified and quantified by NMR, including amino acids (611.1 +/- 36.5 mg/100 g FW), carbohydrates (2801.4 +/- 33.7 mg/100 g FW), lipids (702.7 +/- 28.2 mg/100 g FW), and saffron-specific compounds such as crocin (596.6 +/- 21.5 mg/100 g FW), picrocrocin (1126.3 +/- 18.9 mg/100 g FW), safranal (398.4 +/- 14.8 mg/100 g FW), and crocetin (13.4 +/- 0.4 mg/100 g FW). Targeted fractionation further allowed the identification of kaempferol 3-O-sophoroside (15.44 +/- 0.61% w/w in dry ethanolic extract) and 3-hydroxy-gamma-butyrolactone. Overall, the results highlight the rich metabolite composition of saffron production waste and support its potential reuse as a valuable source of functional ingredients within a circular economy framework.

The overuse of chemical pesticides has accelerated the spread of resistant pathogen strains and raised major human and environmental health concerns, urging the search for sustainable alternatives to control crop diseases. Here, we show that foliar treatments with an aqueous extract of the mass cultivated microalga Cylindrotheca closterium (AEC), obtained without the use of chemical solvents, protect plants against the fungal pathogen Botrytis cinerea, causal agent of grey mould. When sprayed on leaves, AEC suppressed disease symptoms in the model plant Arabidopsis thaliana, as well as in crops like tomato, pepper, and eggplant. This effect persisted for at least one week after treatment, providing long-lasting protection without impairing plant growth and fitness. Notably, AEC appears to exert its protective action by increasing leaf surface hydrophilicity, causing a significant and dose-dependent reduction of water contact angle that correlates to impairment of early stages of B. cinerea infection. Spectroscopic and microscopic analyses indicated that AEC contains significant amounts of Si, as well as polysaccharides, proteins, and other amphiphilic molecules potentially able to modify the physicochemical properties of the leaf surface. Extract fractionation showed that this effect likely arises from the combined action of multiple constituents. By acting directly on the physical properties of the leaf surface, AEC is a promising candidate for novel, sustainable products for crop protection.

Foundries represent complex exposure scenarios where metals, particulate matter, and combustion by-products coexist, posing potential cumulative biological effects. Urinary metabolic profiles from 64 foundry workers and 78 residents living in surrounding areas were investigated using multivariate statistical modeling. Differences in urinary metabolite patterns were observed between the two groups, including lower levels of several amino acids (e.g., valine, alanine, tyrosine, and tryptophan) and tricarboxylic acid intermediates (e.g., citrate and succinate), together with higher levels of selected branched-chain amino acid catabolites (e.g., 3-hydroxyisobutyrate and erythro-2,3-dihydroxybutyrate) in workers. Variations in gut microbiota-related metabolites, such as phenylacetylglycine and p-cresol sulphate, were also detected. Based on these metabolic patterns, potential molecular mechanisms related to energy metabolism, oxidative stress and host-microbiome interaction are discussed as interpretative hypotheses. The comparison between workers and residents was interpreted, taking into account differences in demographic and lifestyle characteristics between groups. Overall, the results indicate that occupational exposure in foundries is associated with measurable differences in urinary metabolic profiles, demonstrating that the applied NMR-based metabolomic strategy is capable of capturing early biological effects and supporting its potential as a non-invasive and holistic biomonitoring tool for evaluating the health impact of complex occupational exposures.

During the last decades, polysaccharides have emerged as promising molecules with valuable pharmacological properties. Within this vein, this study aimed to characterize polysaccharides derived from the pulp of Opuntia stricta (Haw.) Haw (POS), with particular focus on their antioxidant and anti-inflammatory activities. The phytochemical composition of POS was evaluated through an extensive analytical assessment, including structural features and the identification of compounds using gas chromatography-mass spectrometry (GC-MS). The chemical composition analysis showed that POS encompasses 56.73% of polysaccharide, with glucose, mannofuranose, and rhamnose being the shift compounds detected by GC-MS. Fourier-transform infrared and proton nuclear magnetic resonance spectra confirmed the presence of critical functional groups. The antioxidant activity demonstrated that POS effectively scavenged DPPH (1,1-diphenyl-2-picrylhydrazyl) and ABTS (2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic) acid) radicals, exhibited significant reducing power, and inhibited the β-carotene bleaching assay. The in vivo test proved that pre-treatment with POS significantly reduced carrageenan-induced paw edema, lipid peroxidation, and protein oxidation in skin tissues, while improving antioxidant enzyme activities. These findings were further supported by hematological analyses, C-reactive protein levels, and histopathological examination of paw tissue, showing cellular infiltration reduction. In addition, in silico docking investigations against cyclooxygenase (COX)-1 and COX-2 targets were carried out, and significant results were obtained. All these results highlight the outstanding performance of POS as a promising natural antioxidant with anti-inflammatory features, warranting further clinical investigation.

Exposure to brake dust, a component of non-exhaust contribution by vehicular traffic, poses a significant global health threat due to its high content of potentially toxic elements (PTEs). This study employed an innovative approach using untargeted metabolomics on the model organism Drosophila melanogaster adults following larval exposure to brake dust.We exposed or not (control) D. melanogaster larvae in laboratory conditions to brake dust in the food medium at two concentrations: 75 and 750 mg/L. In adult individuals, we assessed both elemental accumulation via ICP-MS analysis (25 elements) as an exposure marker and metabolomic alterations via NMR analysis as an effect marker. Larval brake dust exposure resulted in the significant accumulation of several PTEs (i.e. Bi, Cu, Fe, Sb, Sn, W) in adults and induced a developmental delay at the highest dose (750 mg/L). Metabolomic analysis revealed a distinct stress signature: a generalized decrease in free amino acids (suggesting hyperactive protein synthesis for detoxification/damage repair, including metallothioneins) and a contrasting increase in Glutamine (bolstering glutathione-mediated antioxidant defence). Further signs of metabolic distress included Krebs Cycle disruption and suggested gut microbiota alterations.Overall, our findings demonstrate that larval brake dust exposure causes persistent, system-wide metabolic shifts in adults. The proposed metallomics-metabolomics multi-platform approach using D. melanogaster may represent a powerful tool for advancing toxicological science related to particulate matter health assessment.

The increasing vulnerability of global food systems has led to an interest in the rediscovery of underutilised plant species as alternative and resilient food resources. Among these species, edible weeds such as Cyperus rotundus L., may represent a promising resource. Even though C. rotundus has been considered as one of the most invasive weed species, it produces energy-rich tubers that have been traditionally consumed but remain poorly characterised from a nutritional and technological perspective. This study provides a comprehensive evaluation of the chemical and metabolomic profile, techno-functional properties, digestive behaviour, and phenolic content. Proximate analysis revealed high total dietary fibre content (39.05 ± 1.23 g/100 g FW), dominated by insoluble fibre, followed by starch (15.00 ± 0.53 g/100 g FW), alongside moderate protein levels (8.44 ± 0.14 g/100 g FW). Elemental analysis performed by ICP-MS revealed a mineral profile dominated by nutritionally relevant macronutrients, particularly Ca, K, P, and Mg, and allowed the determination of microelements and trace potentially toxic elements (PTEs), including As, Cd, Pb, and Ni, which were detected only at low concentrations.The untargeted 1H NMR metabolomic analysis identified 37 metabolites, including free sugars, organic acids, fatty acids, sterols, amino acids, and bioactive compounds such as arginine, γ-aminobutyric acid (GABA), and luteolin-7-O-glycoside. Techno-functional analysis showed favourable water- and oil-holding capacities, and stable pasting behaviour, moderate foaming capacity with high foam stability, and suitability for coarse emulsion systems. In vitro digestion demonstrated slow starch hydrolysis, with reducing sugar release closely matching that of the low-digestible starch fraction, suggesting a potential low-glycaemic response. Total phenolic content was 4.71 ± 0.04 mg GAE/g DW. Overall, these findings indicate C. rotundus tubers as a promising candidate for valorisation within modern food and feed systems, where resilient and underutilised species are increasingly essential to face future climate and security challenges.

The phytochemical profile of an Italian accession of Carlina acaulis subsp. caulescens f. typica Cianfaglione is here reported for the first time. Nine secondary metabolites were identified from the aerial parts including one degradation product of chlorophylls, two pentacyclic triterpenoids, one flavonoid, four quinic acid derivatives and one simple organic acid. Their structures were elucidated through NMR and MS analyses. The chemophenetic evaluation revealed the occurrence of two compounds reported for the first time in the genus and three compounds newly identified for the species. However, due to their widespread distribution among plant taxa, these metabolites cannot be considered reliable chemophenetic markers. These phytochemical results have also been compared with those obtained from a recently described new form of the species, finding a few similarities. These results surely demand further in-depth studies on both forms.

Matcha, a finely powdered green tea, has been cherished in Japan for centuries, used in the traditional tea ceremony and nowadays also valued for its health-promoting properties. Cultivated under shaded conditions to enhance chlorophyll production, which gives the typical vibrant green color, matcha is rich in important bioactive compounds, including caffeine, catechins, and theanine. This study analyzes three matcha grades—ceremonial grade 1 (G1), grade 4 (G4), and food grade (FG)—to assess variations in their metabolite profiles. The Bligh–Dyer method was employed to extract polar and non-polar metabolites from organic and hydroalcoholic phases. High-performance thin-layer chromatography (HPTLC) was used for qualitative metabolite analysis, while nuclear magnetic resonance (NMR) spectroscopy was employed for both qualitative and quantitative analyses. Results reveal a decreasing gradient of amino acids and caffeine from grade 1 to food grade, while other metabolites, such as polyphenols, display an increasing trend. These findings suggest that factors such as harvesting time and leaf maturity significantly influence matcha’s chemical composition, providing a scientific basis for its quality differentiation and potential nutraceutical uses.

In this work, the first complete phytochemical analysis ever performed on a European population of Phlomis fruticosa L., led to the identification of twelve metabolites from its leaf ethanolic extract: pheophytin a (1), verbascoside (2), leucosceptoside A (3), apigenin (4), kaempferol (5), 5-hydroxy-8-epi-loganin (6), lamiide (7), penstemoside (8), 5-deoxy-pulchelloside I (9), quinic acid (10), vanillic acid (11) and glycerol (12). Their chemophenetic value was evaluated individuating and even suggesting chemophenetic markers at various levels.

The plastic manufacturing industry has a crucial role in the global economy with a significant impact in a wide range of fields. The chemical risk to which workers are potentially exposed is difficult to characterize and strictly related to both the products and processes adopted. Among the chemicals used, we can cite styrene, phenol, butadiene and phthalates, but nano- and microplastic particles can also be released in the work environment. In this pilot study, we present for the first time an NMR-based metabolomic approach for assessing urinary profiles of workers employed in a plastic manufacturing company. Urine samples from twelve workers and thirteen healthy volunteers were collected and analyzed by NMR spectroscopy. Forty-six urinary metabolites belonging to different chemical classes were univocally identified and quantified. The dataset so obtained was then subjected to multivariate statistical analysis to characterize each profile and highlight any differences. An alteration in some metabolites involved in several pathways, such as amino acid metabolism and NAD metabolism, was found, and a strong impact on gut microflora was also speculated. Ultimately, our work has the objective of adding a tile to the knowledge of biological effects possibly related to occupational exposure even if it is below the threshold limit values.

A standardized classification and description system (coding) of food products allows the analysis of data originating from several sources. The data harmonization process about food composition depends on systematic food description that is indispensable for the acquisition, analysis, and sharing data and information. The availability of well-developed data banks can ensure the efficient management of heterogeneous data, useful for scientific studies and strategic decisions. The rise of harmonized composition data for foods plays a key role in understanding the relationship between human health and diet. Systematic classification and description of food products are used to analyze dietary intake. "Specialty oils", also promoted as "Gourmet" oils, are attracting the attention of consumers for their high amounts of nutritional and nutraceutical components with health-promoting properties. This study aims to codify 50 samples of some vegetable oils, currently sold in physical and online stores in Italy, by applying the two most common classification and description systems: LanguaLTM and FoodEx2. [GRAPHICS]

Background/Objectives: Inflammation and oxidative stress are the main pathogenetic pathways involved in the development of several chronic degenerative diseases. Our study is aimed at assessing the antioxidant and anti-inflammatory activity of hydroalcoholic extracts obtained from wheat and its derivatives. Methods: The content of total phenolic and total flavonoid compounds and antioxidant activity were carried out by ABTS and DPPH assays. The ability of wheat extracts to promote microglia polarization towards an anti-inflammatory phenotype was evaluated analyzing the increased expression of anti-inflammatory markers by real-time qPCR and immunofluorescence assays. Antioxidant activity of all the extracts was evaluated in C. elegans by analyzing ROS levels and the expression of the antioxidant enzymes GST-4 and SOD-3 by real-time qPCR and fluorescence experiments. The expression of key genes involved in the innate immune response and stress resistance pathways—daf-16, sek-1, and pmk-1—was evaluated by real-time qPCR. Results: Wheat extracts showed the ability to polarize microglia cells towards an anti-inflammatory phenotype, even after the addition of LPS. An antioxidant response was detected both in microglia and in Caenorhabditis elegans nematode, where the extracts also implemented an anti-stress resilience response and stimulated the innate immunity. Conclusions: The present study shows that wheat seeds, flour, chaff, and pasta present anti-inflammatory as well as antioxidant activities and may be considered as prospective positive health agents for the preparation of functional foods. Moreover, the valorization of by-products from agricultural and agro-industrial activities would also have significant implications in terms of circular economy.

INTRODUCTION:Pyridoxal 5'-phosphate (PLP), the biologically active form of vitamin B6 is involved in 4% of cellular enzymatic activities and its deficiency is responsible for or contributes to several human diseases. The study of underlying mechanisms is still in its infancy and requires suitable model organisms. In Drosophila the deficiency of vitamin B6 produces chromosome aberrations and hallmarks of human diseases including diabetes and cancer. However, the effects of vitamin B6 deficiency have never been examined at a metabolic level. OBJECTIVES:This study evaluates the metabolic changes in vitamin B6 deficient Drosophila larvae with the aim of validating flies as a suitable model for diseases associated to vitamin B6 deficiency. METHODS:To induce vitamin B6 deficiency we fed Drosophila wild type larvae with 4-deoxypyridoxine (4DP), a PLP antagonist. By HPLC analysis we verified that the 4DP treatment was effective in inducing vitamin B6 deficiency. Using an NMR-based metabolomic approach we compared the metabolites in larval extracts from untreated and 4DP-fed larvae. RESULTS:The NMR spectra analysis identified quantitative differences for sixteen metabolites out of forty, including branched chain and aromatic amino acids, glucose, and lipids, thus revealing interesting possible associations with the phenotypes showed by vitamin B6 deficient flies. CONCLUSIONS:Our results validate Drosophila as a suitable model to study in depth the molecular mechanisms underlying human diseases associated with vitamin B6 deficiency and confirmed that 4DP treatment is effective in inducing vitamin B6 deficiency.

In this work, hydrophilic FeOx-AgNPs nanohybrids were obtained by covalent interaction between functionalized maghemite nanoparticles (gamma-Fe(2)O(3)NPs) and silver nanoparticles (AgNPs). An in situ chemical reduction of the AgNO3 precursor was carried out in the presence of sodium 3-mercapto-1-propanesulfonate (3MPS) stabilizer to further improve colloidal stability and aqueous dispersibility of the nanohybrids. The bifunctional linker (3-mercaptopropyl)trimethoxysilane (MPTMS) enabled the gamma-Fe(2)O(3)NPs surface coating through Fe-O-Si chemical bonds, exposing the -SH ending moiety for covalent decoration of AgNPs-3MPS through covalent Ag-S bonds. Two nanohybrids, namely, FeOx-AgNPs_1 and FeOx-AgNPs_10, were obtained by tuning the Fe/Ag weight ratio, resulting in Ag content of 4-15 wt %, as confirmed by inductively coupled plasma optical emission spectrometry (ICP-OES) measurements. The deep characterizations by UV-Vis spectroscopy, dynamic light scattering (DLS) and zeta-potential, far- and mid- Fourier-transform infrared (FTIR) and Raman spectroscopy, high-resolution transmission electron microscopy (HR-TEM), powder X-ray diffraction (PXRD), elemental analysis, and magnetic susceptibility measurements confirmed their colloidal nature, aqueous stability, surface functionalization, and ferromagnetic behavior. Both hybrids were tested as nanoprimers (0.01-100 ppm concentration range) on Sorghum bicolor (L.) Moench Bianca seeds. FeOx-AgNPs_1, containing the lower Ag content, significantly improved the germination rate without phytotoxic effects at lower concentrations (0.01-1 ppm, i.e., 0.0015-0.15 ppm of metallic Ag). H-1 NMR metabolomic analysis revealed a dose-dependent regulation of amino acid and carbohydrate content, indicating an osmotic adjustment mechanism. The results of this research highlight the possibility of combining gamma-Fe(2)O(3)NPs-MPTMS with AgNPs-3MPS in a single covalent hybrid nanostructure, demonstrating their potential within the frame of nanoprimers as a sustainable alternative to conventional agrochemical treatments.

The continuation of the phytochemical analysis to determine the alkaloid content of Vinca difformis subsp. sardoa Stearn, led to the isolation of the further compound vincamajine (1) which was reported from the species for the first time during this study. Its structure was established by means of extensive NMR, IR and MS analyses which are completely reported in this paper for the first time. In addition, the first chemophenetic evaluation about this compound was also carried out evidencing some important results which were fully described and discussed in this paper.

In this study, Minimedusa polyspora and Chaetomium globosum and their metabolites were assessed in vitro for their ability to inhibit growth of Alternaria alternata, Berkeleyomyces basicola, and Botrytis cinerea, gaining insights into their biocontrol mechanisms. A dual culture, an assay for volatile antimicrobial compounds effectiveness (performed in two different conditions), and a culture filtrate antifungal assay were designed to discriminate the involved mechanisms. Moreover, the culture filtrates of these strains were assessed for fungistatic and fungicidal activities (determining also the minimum inhibitory concentration and the minimum fungicidal concentration) and for the occurrence of siderophores. The results show that both M. polyspora and C. globosum inhibited, to different extents, growth of all the pathogens in the plate assays. Both culture filtrates showed fungistatic and fungicidal activities, pointing to the release of diffusible compounds as an involved biocontrol mechanism. Based on the results of this study, M. polyspora and C. globosum are promising bioprotection agents of these phytopathogens and species of interest for further studies aimed at validating their potential in in vivo conditions.

Natural resins are complex mixtures of secondary metabolites produced by many plants in response to stress or injury and have long been used for their antimicrobial, anti-inflammatory, and antioxidant properties. Among resin-producing genera, Commiphora Jacq. (Burseraceae) stands out for the traditional and medicinal relevance of its oleogum resins, commonly known as myrrh. In this study, we investigated, for the first time, the non-volatile fraction of the oleogum resin of Commiphora ornifolia (Balf.f.) J.B.Gillett, which is an endemic species of Socotra Island. Ethanol extraction followed by chromatographic and spectroscopic analysis (HPLC-DAD, NMR, HRMS) led to the isolation of (+)-yangambin, a furofuran lignan not previously reported in this species. Quantitative analysis showed yangambin to be present in all eight resin samples analyzed, at concentrations ranging from 3.50 (±0.02) to 9.05% (±0.19) of the ethanol extract. In addition, the analysis of the hydrolyzed polysaccharide fraction revealed the presence of arabinose, rhamnose, galactose, and galacturonic acid. These preliminary findings highlight the phytochemical richness of C. ornifolia oleogum resin and suggest the presence of other potentially bioactive compounds. The presence of yangambin, known for various pharmacological activities, supports further phytochemical and biological studies on this largely unexplored species.

Polyporus umbellatus (Pers.) Fr. (Sin. Dendropolyporus umbellatus (Pers.) Jülich) is an edible and medicinal mushroom in the family Polyporaceae (phylum Basidiomycota). Widely distributed in the Northern hemisphere, it is reported for the first time its presence in central Italy, Lazio. Even though the known history of usage in traditional medicine of Polyporus umbellatus, the entire phytochemical profile of both the aqueous and organic extract has not been yet analysed, also specifically from sample of non-Asian origin. In this perspective, it is important to evaluate the presence of other possible bioactive compounds and investigate the quantities of metabolites with a nutraceutical impact. High resolution NMR spectroscopy with 1H-NMR,1H-1H TOCSY, and 1H-13C HSQC was employed, finding 45 metabolites in both aqueous and organic extract, identifying and quantifying compounds of interest for nutrition and human health.