Buffalo milk represents one of the most interested dairy products involved in adulteration practice, as the current yield does not satisfy the increasing demand of the market. The development of an analytical system able to identify adulteration, defending manufacturers/retailers as well as consumers, represents an important challenge for the entire scientific community and national authorities involved in controls. In this study, an analytical system based on an easy-to-use device and chemometric tools was proposed for a rapid screening of the raw material, the buffalo milk. Especially, a spectroscopic method was optimized for the analysis of pure raw material and buffalo milk after adulteration with goat milk, cow milk and water. Spectra were studied by techniques of multivariate statistical analysis. After an explorative investigation of the spectroscopic results, prediction models were validated. The Partial Least Squares-Discriminant Analysis (PLS-DA) model provided accuracy higher 93.7 % and the Soft Modeling Class Analogy (SIMCA) model showed a sensitivity never lower than 91.3 %. The Partial Least Squares regression (PLSr) model ensured a rapid assessment of contamination, providing an error of prediction (RMSEP) never higher than 5.2 %. The proposed MicroNIR/Chemometric system proved to be a rapid and sensitive tool for real-time investigation of dairy products at any farm levels.

The surface material’s nature can influence the formation of biofilms. Environmentally friendly materials such as linoleum, derived from organic sources, have emerged to address the need to balance ecological requirements with practical considerations, particularly in sectors where hygiene is of critical importance, such as sports and healthcare. Nevertheless, even with appropriate utilization, these materials can deteriorate over time, resulting in the proliferation of harmful microbes. Metagenomic analyses were conducted to identify the microbiota responsible for the chromatic variation (n = 4) observed on a linoleum sample immersed in water. Subsequently, the data were correlated with spectroscopic analyses via microNIR. The preliminary investigations did not establish the role of abiotic components in the processes of surface discoloration. The bacterial microbiota formed on the surfaces was characterized, indicating a potential biotic role in the degradation of linoleum. Data exploration obtained from the spectroscopic acquisitions through principal component analysis produced a clustering of the data matrix into four subgroups, corresponding to the four chromatic variations. The preliminary data appear to indicate the degradation mechanisms to which materials of organic origin are subject. Furthermore, they suggest that the personalized functionalization of such materials could support effective replacement from a One Health perspective of traditional materials.

Understanding the connection between ocean health and human health is currently limited and fragmented, calling for transdisciplinary research and strategic action. The contribution of public health experts alongside marine scientists are essential for a comprehensive understanding of the health-environment-climate nexus in a Planetary Health perspective. This paper proposes a novel Model for a standing Global Partnership, the SeA Care project. This initiative aims to align efforts within the framework of the Sustainable Development Goals merging the principles of Planetary Health with the “One Water” approach. By doing so it seek to foster the development and assessment of new strategies for oceanwide surveillance focusing on adaptation, mitigation and prevention.

Mass spectrometry (MS) and coupled gas chromatography-mass spectrometry (GC-MS) are globally recognized as the primary techniques for the analysis of gases or vapors due to their selectivity, sensitivity, accuracy, and reproducibility. When thermal stress is applied, vapors or gases are released as a result of the reactions and changes that occur. The analysis of these gases during the thermally induced reaction is scientifically referred to as evolved gas analysis (EGA), which is essential for confirming the occurrence of the induced reactions. Pyrolyzers, thermobalances, or simple heaters can increase the temperature of the analyzed samples according to a programmed and software-managed ramp, allowing for control over both the heating rate and isothermal stages. The atmosphere can also be varied to simulate pyrolysis or thermo-oxidative processes. This way, each induced reaction generates a unique evolved gas, which can be linked to a theoretically hypothesized mechanism. Mass spectrometry (MS) and coupled gas chromatography–mass spectrometry (GC-MS) are fundamental analytical methods used for on-line thermally induced evolved gas analysis (OLTI-EGA).

This study investigated the bioaccumulation patterns of polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and per- and polyfluoroalkyl substances (PFASs) in the liver and muscle tissues of wild boars (n = 39) and domestic pigs (n = 38) from Northern Italy. This research addressed a critical gap in our understanding of how different ecologies and diets influence the uptake of persistent organic contaminants in two closely related species, one domestic and one wild. Significant differences in contaminant profiles were observed, largely attributable to distinct exposure routes and feeding behaviors. Wild boars displayed different quantities and families of environmental contaminants, with higher PCB levels in muscle and PFASs in liver. Conversely, domestic pigs exhibited markedly higher PAH concentrations, primarily linked to contaminated feed in controlled agricultural settings. The liver consistently demonstrated a central role in toxicant retention across both species. Notably, concentrations of several regulated PFAS compounds in both wild and farmed animals exceeded EU maximum levels (sum of PFOS, PFOA, PFNA, and PFHxS: 1.3 µg/kg), raising significant food safety concerns. These findings underscore the critical need for continuous environmental biomonitoring, stricter control of contaminant sources in agriculture, and updated risk assessments for both wild and domestic meat products to protect animal welfare and human health.

A novel challenging purpose in probiotic market, is represented by the possibility of including probiotics into nutraceutical products in order to produce probiotic capsules with a dual impact on human health. Based on this incoming demand, this work provide a novel microencapsulation strategy to introduce probiotic into nutraceutical products claimed as food supplements. Spray congealing encapsulation of Lactic Acid Bacteria (LAB) was used to obtain an innovative formulation exhibiting a good storage stability of probiotics (not less than 109 CFU/ cps) in not refrigerated conditions and the viability was evaluated for a period of 12 months. The results of the analytical characterization of the microparticles performed by Thermogravimetric Analysis, the enumeration of the living cells and the Scanning Electron Microscopy (SEM) permitted to evaluate the efficiency of the microencapsulation process and to collect probiotic powder with the suitable morphology and not exceeding 400 mu m as average diameter, in order to be included into capsules as oral dosage form.

This study aimed to investigate the exposure of wild boars and swine from semi-extensive farms in the same area to essential and non-essential elements, measuring their concentration in liver and muscle. Furthermore, the study explored the influence of factors such as sex, age, and the sampling location on wild boars. Higher liver element concentrations were observed in both wild boars and swine. Geographical comparisons revealed minor differences. Young wild boars showed significantly higher Cu, Se, Cd, and Cr levels, while older subjects exhibited elevated Mn levels, reflecting age-related element absorption variations. No significant sex-based variations were noted. Comparing wild boars to swine, wild boars had more non-essential elements due to their foraging behavior and a larger home range. Conversely, swine exhibited a greater prevalence of essential elements, potentially resulting from dietary supplementation.

Sulforaphane is a chiral phytochemical with chemopreventive properties. The presence of a stereogenic sulfur atom is responsible for the chirality of the natural isothiocyanate. The key role of sulfur chirality in biological activity is underscored by studies of the efficacy of individual enantiomers as chemoprotective agents. The predominant native (R) enantiomer is active, whereas the (S) antipode is inactive or has little or no biological activity. Here we provide an enantioselective high-performance liquid chromatography (HPLC) protocol for the direct and complete resolution of sulforaphane and its chiral natural homologs with different aliphatic chain lengths between the sulfinyl sulfur and isothiocyanate group, namely iberin, alyssin, and hesperin. The chromatographic separations were carried out on the immobilized-type CHIRALPAK IH-3 chiral stationary phase with amylose tris-[(S)-methylbenzylcarbamate] as a chiral selector. The effects of different mobile phases consisting of pure alcoholic solvents and hydroalcoholic mixtures on enantiomer retention and enantioselectivity were carefully investigated. Simple and environmentally friendly enantioselective conditions for the resolution of all chiral ITCs were found. In particular, pure ethanol and highly aqueous mobile phases gave excellent enantioseparations. The retention factors of the enantiomers were recorded as the water content in the aqueous-organic modifier (methanol, ethanol, or acetonitrile) mobile phases progressively varied. U-shaped retention maps were generated, indicating a dual and competitive hydrophilic interaction liquid chromatography (HILIC) and reversed-phase liquid chromatography retention mechanism on the CHIRALPAK IH-3 chiral stationary phase. Finally, experimental chiroptical studies performed in ethanol solution showed that the (R) enantiomers were eluted before the (S) counterpart under all eluent conditions investigated.

Limited or absent activity of the enzyme α-galactosidase A (α-Gal A), due to mutation in the related gene on the X chromosome, leads to the development of a rare hereditary and genetic disease known as Fabry disease (FD). This pathology involves a progressive accumulation in various organs of the substrates of the enzyme e.g., globotriaosylceramide (Gb3) and its deacylated form, globotriaosylsphingosine (Lyso-Gb3), suggesting these molecules as biomarkers of Fabry disease. The present paper describes the development of an analytical strategy for the identification and quantification of Gb3 and Lyso-Gb3, in serum and blood samples by using liquid chromatography (LC) coupled to mass spectrometry in multiple reaction monitoring (MRM/MS) ion mode. The best experimental conditions were obtained by extracting the glycolipids with chloroform/methanol/H2O (2/1/0.3) and by separating them on a C4 column with a linear gradient (A: H2O with 2 mM ammonium formate. B: methanol with 1 mM ammonium formate, both acidified with 0.2% formic acid). The best transitions (a combination of precursor and fragment ions—m/z) were 786.8 m/z > 268.3 m/z for Lyso-GB3, 1137.3 m/z > 264.3 m/z for Gb3, 1039.3 m/z > 264.4 m/z for N-heptadecanoyl-ceramide trihexoside, and 843.5 m/z > 264.3 m/z for N-glycinated lyso-ceramide trihexoside, the latter being used as an internal standard. The developed method provided a reliable, fast, and effective procedure for direct measurements of GB3 and Lyso-GB3 in serum and blood for diagnosis of Fabry disease, suggesting this method as a complementary assay to the current enzymatic test. Therefore, this approach could open new insights into the clinical diagnostics of lysosomal storage disorders.

The interest in the quality control of the raw materials, intermediates, and final products, as well as production methods, of beer has increased significantly in recent decades due to the needs and expectations of consumers. Increasing in the industrialization and globalization of beer supply chains led to a need for novel analytical tools suitable for the rapid and reliable characterization of the materials involved. In this study, an ultracompact instrument operating in the NIR region of the spectrum, microNIR, was tested for the chemical investigation of barley malts. The essential raw materials for brewing require careful control since they deeply affect the characteristic flavor and taste of the final products. Therefore, a robust prediction model able to classify base and specialty barley malts was developed starting from NIR measurements. Soft Independent Class Analogy (SIMCA) was selected as the chemometric technique for the optimization of two prediction models, and ground and sieved materials were investigated using spectroscopy. The microNIR/chemometric approach proposed in this study permitted the correct prediction of the malt samples included in the external validation set, providing false positive and false negative rates no higher than 3.41% and 0.25%, respectively, and confirming the feasibility of the novel analytical platform.

BackgroundRecently, environmental pollution has become a significant concern for human, animal, and environmental health, fitting within the “One Health” framework. Among the various environmental contaminants, per- and polyfluoroalkyl substances (PFASs) have gathered substantial attention due to their persistence, bioaccumulation, and adverse health effects. This study aimed to compare the levels of 12 PFASs in the fur, liver, and muscle of wild roe deer to evaluate the feasibility of using fur as a non-invasive biomonitoring matrix.MethodsA total of 20 male and 20 female roe deer aged between 12 and 24 months were randomly sampled from a hunting area in Northern Italy. Samples of fur, muscle, and liver were collected post-mortem, and PFAS concentrations were measured using a validated UHPLC-HRMS method.Results and discussionThe results indicated significant differences in PFAS concentrations among the three matrices. Fur, although easier to sample and store, showed highly variable PFAS levels, with different detection frequencies compared to the muscle and liver. PFASs such as PFHxA were more frequently detected in fur than in the liver and muscle, while compounds such as PFBA, PFPeA, PFHpA, PFDA, PFHxS, 6-2 FTS, and 8-2 FTS were less frequently detected in fur. In conclusion, while fur presents many practical advantages for biomonitoring, such as non-invasive sampling and stability, its use is complicated by varying detection frequencies and concentration levels. These aspects, together with the use of a single sampling technique, can be considered a limitation of the study. Notably, compounds such as PFOA, PFNA, and PFOS showed partially similar detection frequencies across the matrices, suggesting potential interest for further research. This study offers new perspectives on the use of fur for environmental monitoring, highlighting the need for more extensive research to understand the relationship between PFAS concentrations in fur and other biological matrices. Future studies should focus on methodological improvements in extraction and quantification techniques for PFASs in fur to enhance their reliability as a biomonitoring tool.

Perfluoroalkyl substances (PFASs) are a heterogeneous group of fluorinated synthetic compounds characterised by the presence of a hydrophobic carbonyl chain at different fluorination rates and by a terminal hydrophilic group. Because of their persistence and mobility, PFASs have been widely detected in ecosystems and living organisms, leading to their classification as persistent organic pollutants (POPs). Hence, monitoring the PFASs content in solid waste meant for disposal in non-hazardous landfills can be crucial, since leachate can pose a significant pollution threat to farmlands and aquifers. Therefore, a QuEChERS and SPE pretreatment with HPLC-MS/MS detection method for 10 different PFASs in solid waste samples was developed in this study. Different sample preparation approaches have been evaluated, taking into account the lack in the literature of this complex matrix. An innovative application using the Captiva EMR cartridge for the clean up (designed to be applied to lipidic matrix) was proposed and a multiresidual HPLC-MS/MS method for the analysis of PFASs in internal waters was extended to the investigation of non-lipidic samples as solid wastes. The method was then validated through 6 blanks and 6 spiked samples, according to the UNI EN ISO/IEC 17025. The optimized method showed satisfactory performance with recoveries ranging from 89.8 % to 106.5 % and with LOD and LOQ ranging between 0.0023 - 0.09 mu g/L and 0.006 - 0.13 mu g/L, respectively, for each of the PFASs under consideration. In addition, this approach demonstrated to be reliable and time consuming due to its capability for determining PFASs in waters and in solid wastes simultaneously in a single chromatographic run.

The analytical study described in this work, based on NIR spectroscopy with a handheld device, allowed the development of a chemometric prediction model that has been validated for the objective evaluation of the ripening of olive drupes. The miniaturized, portable NIR spectrometer is proposed here as an easy-to-use sensor able to estimate the best harvesting time for ripening of olive drupes. The MicroNIR/chemometrics approach was developed for on-site identification of olive drupe ripening directly on plants, avoiding collection and successive laboratory analysis steps. A supporting parallel characterization by chromatographic techniques validated the spectroscopic prediction. The novelty of this approach consists in the possibility of investigating the olive drupe maturation point by collecting spectra in the near-infrared region and processing them using a chemometric model. The fast and accurate device allows one to easily follow the spectrum profile changes of olive drupes during ripening, thus preserving the fruits from being harvested too early or too late. The results of this study demonstrate the possibility of using the MicroNIR/chemometrics approach to determine the optimal ripening time of olives regardless of the plant variety, age and cultivation location. The results consequently demonstrated that the MicroNIR/chemometrics approach can be proposed as a new method to perform on-site evaluation of ripening by a single-click device. It can be conveniently used by any operator, who does not necessarily have to be expert but must simply be trained to use spectroscopy and a prediction model.

Recently, there has been a growing interest in producing functional foods containing encapsulated probiotic bacteria due to their positive effects on human health. According to their perceived health benefits, probiotics have been incorporated into a range of dairy products, but the current major challenge is to market new, multicomponent probiotic foods and supplements. Nevertheless, only a few products containing encapsulated probiotic cells can be found as non-refrigerated products. In this work, spray drying technology was investigated in order to produce an innovative nutraceutical formulation based on lactic acid bacteria (LAB), and was able to ensure a good storage stability of probiotics (no less than 109 CFU/cps) in non-refrigerated conditions. Probiotic-loaded microparticles from spray drying experiments were produced under different conditions and compared by thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and the enumeration of the number of viable cells in order to identify the formulation exhibiting the most promising characteristics. Results from the dissolution test revealed that the optimized formulation provides a suitable amount of living cells after digestion of microparticles stored for 12 months at room temperature and confirmed that the microencapsulation process by spray drying ensures a good protection of probiotics for nutraceutical purposes.

Rosuvastatin (RSV) is a well-established lipid-lowering drug. RSV is susceptible to degradation under various stress conditions and forms two cyclic derivatives by a radical-mediated photolytic mechanism. On a structural basis, these epimeric compounds (reported as FP-B in the European Pharmacopeia monograph Rosuvastatin tablets) retain the configuration of the stereogenic carbons of RSV (3R,5S) and have opposite absolute configurations at the third stereogenic center. Herein, we report the kinetics of formation and the complete structural characterization, including the assignment of the absolute configuration, of each epimer collected after HPLC separation on a chiral stationary phase. The stereochemistry of the epimers was determined by comparison of the experimental circular dichroism data with the corresponding theoretical values. Kinetic studies revealed that RSV degrades completely to FP-B within 3 h at room temperature. Furthermore, through a multi-disciplinary approach involving chromatography (HPLC and UHPLC), circular dichroism (CD), nuclear magnetic resonance (NMR) spectroscopy and mass spectrometry (MS), it was demonstrated that FP-B in turn degrades to the lactones under the mild acidic conditions of the chromatographic mobile phase. The ability of RSV to form multiple degradation products may affect the quantification of RSV-related substances and draw attention to potentially toxic RSV-like species in the environment.

Due to its excellent properties, poly(ethylene terephthalate) (PET) is one of the most produced and consumed polymers. Among plastics, it represents the main contributor to environmental pollution. Following the circular economy model, the chemical upcycling of PET reduces the amount of waste generated and transforms it into high-value products. The depolymerization of poly(ethylene terephthalate) into oligomers or monomers leads to forming a library of reactive molecules involved in different polymerization processes to obtain compounds with improved properties. Herein, several β-hydroxy amines were synthesized and used for the chemical recycling of water bottle waste by an environmental benefit aminolysis process to get very useful new terephthalamide diol monomers. The recycled diol monomers were subsequently exploited to synthesize poly(urethane acrylates) (PUAs) UV-curable coatings, and their chemical, thermal and mechanical characterizations were performed. The results show the great potential of the developed synthesis protocols to obtain PUAs with final properties that can be modulated to meet the requirements of different applications.

The rheological properties of blood play an important role in regulating blood flow in micro and macro circulation. In thalassemia syndromes red blood cells exhibit altered hemodynamic properties that facilitate microcirculatory diseases: increased aggregation and reduced deformability, as well as a marked increase in adherence to the vascular endothelial cells. A personalized approach to treating thalassemia patients (transfusions, iron chelation, and splenectomy), has increased patients' life expectancy, however they generally present many complications and several studies have demonstrated the presence of high incidence of thromboembolic events. In this study the hemorheological profiles of thalassemia patients have been characterized to point out new indices of vascular impairment in thalassemia. Plasma viscosity, blood viscosities at low and high shear rates (η1 and η200, respectively), erythrocyte aggregation index (η1/η200), and the erythrocyte viscoelastic profile (elastic modulus G', and viscous modulus G") have been studied in transfusion-dependent and non-transfusion-dependent thalassemia patients. Moreover, the levels of inflammation biomarkers in thalassemia have been evaluated to investigate a relationship between the biomarkers, the disease severity and the rheological parameters. The biomarkers studied are the main components of the immune and endothelial systems or are related to vascular inflammation: cytokines (IL-2, IL-6, IL-10, IL-17A, TNF-alpha), chemokines (IL-8, MIP-1alpha), adipocytokines (leptin and adiponectin), growth factors (VEGF, angiopoietin-1), adhesion molecules (ICAM-1, VCAM-1, E-selectin, L-selectin), and a monocyte/macrophage activation marker (CD163). This study shows that transfusion-dependent thalassemia patients, both major and intermedia, have blood viscosities comparable to those of healthy subjects. Non-transfusion-dependent thalassemia intermedia patients show high blood viscosities at low shear rates (η1), corresponding to the flow conditions of the microcirculation, an increase in erythrocyte aggregation, and high values of the elastic G' and viscous G" modules that reflect a reduced erythrocyte deformability and an increase in blood viscosity. Levels of cytokines, chemokines and adhesion molecules are different in transfusion- and non-transfusion dependent patients and positive correlations between η1 or η1/η200 and the cytokines IL-6 and IL-10 have been observed. The evaluation of the hemorheological profiles in thalassemia can provide new indicators of vascular impairment and disease severity in thalassemia in order to prevent the onset of thromboembolic events.

Background: Brewer’s spent grain (BSG) is one of the main by-products of beer industry, little used because of its high moisture making it difficult to transport and store. Mainly used as animal feed and for energy production, the agro-industrial waste have recently attracted attention as source of bioactive compounds, with potential applications in many sectors as food, nutraceutical, pharmaceutical, cosmetic, food packaging. The present work focuses on BSG as potential source of valuable small-size bioactive compounds. Methods: Laboratory-made BSG was obtained by using four base malts for mashing. After drying, BSG was eco-friendly extracted with water and the extracts analyzed by untargeted ElectroSpray Ionization (ESI)-Mass Spectrometry (MS)/Mass Spectrometry (MS) (ESI-MS/MS) infusion experiments and by targeted High Performance Liquid Chromatography-PhotoDiodeArray-ElectroSpray Ionization-Mass Spectrometry (HPLC-PDA-ESI-MS) in Selected Ion Recording (SIR) mode analysis, to investigate the metabolic profile, the phenolic profile, the individual phenolic content, and tryptophan content. Aqueous extracts of malts and wort samples were also analyzed for a comparison. Data were statistically analyzed by ANOVA test. An explorative analysis based on Principal Component Analysis (PCA) was also carried out on malts, wort and threshes, in order to study correlation among samples and between samples and variables. Results: The untargeted ESI-MS/MS infusion experiments provided the mass spectral fingerprint of BSG, evidencing amino acids (γ-aminobutyric acid, proline, valine, threonine, leucine/isoleucine, lysine, histidine, phenylalanine and arginine) and organic and inorganic acids (pyruvic, lactic, phosphoric, valerianic, malonic, 2-furoic, malic, citric and gluconic acids), besides sugars. γ-Aminobutyric acid and lactic acid resulted predominant among the others. The targeted HPLC-PDA-ESI-MS in SIR mode analysis provided the phenolic profile of the polar fraction of BSG, evidenced tryptophan as the main residual metabolite in BSG (62.33–75.35 μg/g dry BSG), and catechin (1.13–4.24 μg/g dry BSG) as the representative phenolic antioxidant of not pre-treated BSG samples. The chemometric analysis of the individual compounds content in BSG, malt and wort evidenced similarities and differences among the samples. Conclusions: As main goal, the phytochemical characterization of BSG from base malts highlighted BSG as a potential source of small biomolecules, as tryptophan and catechin, besides γ-aminobutyric acid and lactic acid, opening to new perspectives of application for BSG. Strategies for their recovery are a future challenge. Moreover, ESI-MS/MS analysis was confirmed as a powerful tool for fast characterization of complex matrix. Last, results obtained by chemometric elaboration of data demonstrated the possibility to monitor a small number of molecules to ensure the quality of a final product.

The on-line thermally induced evolved gas analysis (OLTI-EGA) is widely applied in many different fields. Aimed to update the applications, our group has systematically collected and published examples of EGA characterizations. Following the recently published review on EGA-MS applications, this second part reviews the latest applications of Evolved Gas Analysis performed by on-line coupling heating devices to infrared spectrometers (EGA-FTIR). The selected 2019, 2020, 2021 and early 2022 references are collected and briefly described in this review; these are useful to help researchers to easily find applications that are sometimes difficult to locate.