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Whole wheat is an exceptional source of phenolic compounds representing a promising phytochemical class to prevent diet-related chronic diseases thanks to its antioxidant activities. The present work reports the phenolic profile, the antioxidant capacity, the antimicrobial activity and the effect on Lactobacillus brevis growth of eight whole flours obtained from four ancient and modern wheat genotypes of Italian Triticum genus. Total phenolic content (TPC) and total flavonoid content (TFC) were quantified, and antioxidant activities were assessed using oxygen radical absorbance capacity (ORAC) and 2,2-diphenyl-1-picrylhydrazyl (DPPH) in vitro tests. HPLC-DAD/FLD was used to detect the presence of phenolic compounds. Moreover, antimicrobial activity of whole flour extracts against some potentially pathogenic Gram negative and Gram positive bacteria and the effect of extracts on Lactobacillus brevis growth were assessed. Results showed quantitative differences (p L. brevis was stimulated. The principal component analysis (PCA) confirmed that the phenolic profile and the antioxidant activities were influenced by the genotypic characteristics of studied varieties, suggesting that the ancient Saragolla stand out for the most interesting phenolic profile. Overall, this research emphasizes how ancient and modern Italian Triticum spp. grains must be investigated to select the grains richer in bioactive compounds. Graphical abstract

Background. Salivary metabolomics is garnering increasing attention in the health field because of easy, minimally invasive saliva sampling. Dihydrouracil (DHU) is a metabolite of pyrimidine metabolism present in urine, plasma, and saliva and of fluoropyrimidines-based chemotherapeutics. Its fast quantification would help in the identification of patients with higher risk of fluoropyrimidine-induced toxicity and inborn errors of pyrimidine metabolism. Few studies consider DHU as the main salivary metabolite, but reports of its concentration levels in saliva are scarce. We propose the direct determination of DHU in saliva by reversed-phase high-performance liquid chromatography (RP-HPLC-UV detector) as a simple, rapid procedure for non-invasive screening. Methods. The method used was validated and applied to 176 saliva samples collected from 21 nominally healthy volunteers and 4 saliva samples from metastatic colorectal cancer patients before and after receiving 5-fluorouracil chemotherapy. Results. DHU levels in all samples analyzed were in the μmol L−1 range or below proving that DHU is not the main metabolite in saliva and confirming the results found in the literature with LC-MS/MS instrumentation. Any increase of DHU due to metabolism dysfunctions can be suggestive of disease and easily monitored in saliva using common, low-cost instrumentation available also for population screening.

Currently, there is an increasing interest in the development of HVAC systems based on solid desiccant materials to achieve efficient and affordable air dehumidification and humidification processes. Many research efforts deal with the development of novel composite materials suitable to manufacture such devices. In this work we present a novel silica gel-based desiccant compound, which can be used to prepare different products, such as sheets, monolithic components, and coatings. The proposed formulation is based on a combination of silica gel, sodium polyacrylate, vinyl glue and polypropylene fibers. The preparation procedure of the sorbent material and its characterization (adsorption capacity, morphology and surface analysis, mechanical properties by pull-off test, structural and thermal stabilities of new and aged samples and volatile compounds emissions) are described in detail. A small-scale prototype has been also manufactured and experimentally tested under typical operating conditions of air dehumidification processes. Results show that the proposed material has a suitable sorption capacity (maximum water uptake equal to 0.32 kg kg-1), good mechanical properties (pull adhesion strength around 2.74 MPa) and stability (decomposition threshold of 400 °C). The performances achieved by the prototype are comparable with those of a reference silica gel packed bed system, highlighting that the desiccant material performs adequately also at system scale.

Background. In IWCLL guidelines, progressive splenomegaly and lymphadenopathy are signs of active disease. In this study, we have tested the hypotheses if US could be a reliable tool for both superficial lymphnodes (SupLNs) and splenic assessment in chronic lymphocytic leukemia (CLL) patients. Methods. We enrolled N = 75 patients. SupLN and the spleen were assessed by two independent physicians (M1 and M2) by palpation and by a third physician (M3) with ultrasound sonography (US) using two different sonographers (US1 and US2). The results of M1 vs. M2 assessment, US1 vs. US2, palpation vs. US were compared. The echostructure of N = 1037 SupLN and of the spleen was also investigated. Results. The dimensions of SupLNs assessed by MD1 vs. MD2 were statistically discordant. Splenic size was concordant. There was concordance between US1 and US2 SupLN and splenic assessment. US found a higher number of pathological SupLN (Cohen’s Kappa < 0.1) than palpation, which misses remarkable-sized SupLNs. LN echostructure and splenic involvement patterns were described. Conclusions. US is a reliable, radiation-free tool useful in clinical practice to assess SupLN and splenic involvement in CLL.

Fibrous composites of tetraethylortosilicate (TEOS)/polyvinylpyrrolidone (PVP) have been successfully prepared by a sol-electrospinning process and characterized by ATR-FTIR spectroscopy, and the spectroscopic features correlated with their morphology and thermal stability. PVP is a polymer with water adsorption capability and the TEOS addition allowed to increase the thermal stability of microfibers. The spectroscopic analysis of the impact of the silica-based reinforcing phase along with morphological and thermal analysis have demonstrated that TEOS in PVP/ethanol system may interfere with the evaporation of water and ethanol during ES process and with the final capacity of the material of adsorbing water. The elucidation of these mechanisms may help in the design of hybrid, organic-inorganic microfibers materials for specific applications, as adsorbent materials for heat pumps.

A fixed duration of venetoclax-rituximab (VenR) resulted in a significant benefit of both PFS and in the attainment of an undetectable minimal residual disease (uMRD) compared with bendamustine-rituximab in relapsed/refractory (R/R) chronic lymphocytic leukemia (CLL) patients. The 2018 International Workshop on CLL guidelines, outside the context of clinical trials, suggested ultrasonography (US) as a possible imaging technique to evaluate visceral involvement, and palpation to evaluate superficial lymph nodes (SupLNs). In this real-life study we prospectively enrolled N = 22 patients. Patients were assessed by US, to determine nodal and splenic response in R/R CLL patients treated with a fixed duration VenR. We found an overall response rate, complete remission, partial remission, and stable disease, of 95.4%, 68%, 27.3%, and 4.5%, respectively. Responses were also correlated with risk categories. The time to response, and the time to clearance of the disease in the spleen, in abdominal LN (AbdLNs), and in SupLNs were discussed. Responses were independent from LN size. The correlation between response rate with MRD were also investigated. US allowed to detect a substantial CR rate correlated with uMRD.

In order to increase their sustainability, antimicrobial renewable molecules are fundamental additions to consumer goods. Rosmarinic acid is extracted from several terrestrial plants and represents an effective anti-microbial agent. Ulvan, extracted from algae, is an anti-microbial polysaccharide. The present review is dedicated to discussing the sources and the extraction methodologies for obtaining rosmarinic acid and ulvan. Moreover, the preparation of bioanosystems, integrating the two molecules with organic or inorganic substrates, are reviewed as methodologies to increase their effectiveness and stability. Finally, the possibility of preparing functional biomaterials and anti-microbial final products is discussed, considering scientific literature. The performed analysis indicated that the production of both molecules is not yet performed with mature industrial technologies. Nevertheless, both molecules could potentially be used in the packaging, biomedical, pharmaceutical, cosmetic, sanitary and personal care sectors, despite some research being required for developing functional materials with specific properties to pave the way for many more applications.

(1) Background: Neutropenic enterocolitis (NEC) is a life-threatening complication following chemotherapy with high mortality rates. Early diagnosis is crucial to improve outcomes. We designed a large prospective study employing bedside ultrasonography (US) as a novel approach to allow early diagnosis and prompt treatment to reduce mortality. (2) Methods: NEC was defined as US or computed tomography (CT)-proven bowel wall thickness ≥ 4 mm at the onset of at least one of the following symptoms: fever and/or abdominal pain and/or diarrhea during neutropenia. From 2007 to 2018, 1754 consecutive patients underwent baseline bedside US that was invariably repeated within 12 h from the onset of symptom(s) suggestive of NEC. (3) Results: Overall, 117 episodes of NEC were observed, and overall mortality was 9.4%. Bowel wall thickening was invariably absent in the negative control group. Abdominal pain associated with one or more symptoms correlated with the highest relative risk (17.33), sensitivity (89.7%), specificity (100%), and accuracy (96.2%) for diagnosis. The combination of abdominal pain and fever at onset significantly correlated with worse survival (p &lt, 0.0001, OR 13.85). BWT (p = 0.046), type of therapy (p = 0.049) and blood culture positivity (p = 0.003) correlated with worse survival. (4) Conclusions: Bedside ultrasound is a non-invasive and radiation free imaging technique for early diagnosis of NEC and its prompt treatment significantly reduced mortality.

The European dependencies for raw materials supply from foreign countries have been unquestionably shown by COVID‐19 outbreak and have become particular evident from the slow response to the need for high quality personal protective equipment (PPEs). Among all medical devices, surgical face masks have earned themselves a primary role for the containment of the epidemic. In this context, our work aims at improving the barrier effect of surgical mask by depositing on their external surface a mixture of bioactive compounds, mainly polyphenols, extracted from agronomical sources. The main objective is the integration of the biorefining of agri‐food solid wastes with the potential virucidal properties of the polyphenolic extracts for the treatment of PPEs., The experimental workflow proposed in this work. Vegetable wastes are selected, dried, crush into powder and extracted with 70 % ethanol. The solution is used to cover the surface of surgical face masks and improve their barrier effect against pathogens.

Poultry feathers are among the most abundant and polluting keratin-rich waste biomasses. In this work, we developed a one-pot microwave-assisted process for eco-friendly keratin extraction from poultry feathers followed by a direct electrospinning (ES) of the raw extract, without further purification, to obtain keratin-based bioplastics. This microwave-assisted keratin extraction (MAE) was conducted in acetic acid 70% v/v. The effects of extraction time, solvent/feathers ratio, and heating mode (MAE vs. conventional heating) on the extraction yield were investigated. The highest keratin yield (26 ± 1% w/w with respect to initial feathers) was obtained after 5 h of MAE. Waste-derived keratin were blended with gelatin to fabricate keratin-based biodegradable and biocompatible bioplastics via ES, using 3-(Glycidyloxypropyl)trimethoxysilane (GPTMS) as a cross-linking agent. A full characterization of their thermal, mechanical, and barrier properties was performed by differential scanning calorimetry, thermogravimetric analysis, uniaxial tensile tests, and water permeability measurements. Their morphology and protein structure were investigated using scanning electron microscopy and attenuated total reflection-infrared spectroscopy. All these characterizations highlighted that the properties of the keratin-based bioplastics can be modulated by changing keratin and GPTMS concentrations. These bioplastics could be applied in areas such as bio-packaging and filtration/purification membranes.

A microwave (MW)/deep eutectic solvent (DES)-assisted (MWDA) extraction process for obtaining value-added compounds from chestnut shell waste (CSW) is presented. DESs were used as green solvents featuring both high biomass dissolution ability and good response to MW irradiation. A survey of different acid-based DESs led to the identification of Choline Chloride (ChCl)-oxalic acid as the system most sensitive to experimental design variations, especially when considering the total phenolic content (TPC) and the total mass amount recovered (yield wt%). Hence, the MW absorption properties of ChCl-oxalic acid dihydrate and ChCl-oxalic acid DESs, as single components and in mixture with water, were assessed by the experimental determination of their MW heating response. Moreover, the extraction efficiency for the best MW responding system, ChCl-oxalic acid dihydrate, was evaluated at different MW-irradiation times and extraction temperatures. The isolated polyphenols from CSW were further characterized by HPLC-DAD analysis. Gallic acid, ellagic acid, catechin hydrate and procyanidin B2 were identified and quantified, with their relative ratios varying as a function of the MWDA extraction conditions. Lignin, hemicellulose and cellulose compositions of the solid residues of CSW after the MWDA extraction were assessed using a cross validation model obtained by partial least squares regression (PLS) of their FTIR spectra. The chemometrics results, corroborated by SEM analyses, highlighted the ability of the oxalic acid-based DES to simultaneously remove lignin during polyphenol extraction. Overall, the MWDA extraction process presented here enables the fast, cheap and tunable processing of food waste yielding a high amount of valuable bioactive compounds. This journal is

Metabolomic profiling of cell lines has shown many potential applications and advantages compared to animal models and human subjects, and an accurate cellular metabolite analysis is critical to understanding both the intracellular and extracellular environments in cell culture. This study provides a fast protocol to investigatein vitrometabolites of immortalized hippocampal neurons HN9.10e with minimal perturbation of the cell system using a targeted approach. HN9.10e neurons represent a reliable model of one of the most vulnerable regions of the central nervous system. Here, the assessment of their extracellular metabolic profile was performed by studying the cell culture medium before and after cell growth under standard conditions. The targeted analysis was performed by a direct, easy, high-throughput reversed-phase liquid chromatography with diode array detector (RP-HPLC-DAD) method and by headspace solid-phase microextraction–gas chromatography–mass spectrometry (HS-SPME-GC-MS) for the study of volatile organic compounds (VOCs). The analysis of six different batches of cells has allowed to investigate the metabolic reproducibility of neuronal cells and to describe the metabolic “starting” conditions that are mandatory for a well-grounded interpretation of the results of any following cellular treatment. An accurate study of the metabolic profile of the HN9.10e cell line has never been performed before, and it could represent a quality parameter before any other targeting assay or further exploration.

Saliva is an interesting, non-conventional, valuable diagnostic fluid. It can be collected using standardized sampling device, thus, its sampling is easy and non-invasive, it contains a variety of organic metabolites that reflect blood composition. The aim of this study was to validate a user-friendly method for the simultaneous determination of low molecular weight metabolites in saliva. We have optimized and validated a high throughput, direct, low-cost reversed phase liquid chromatographic method with diode array detection method without any pre- or post-column derivatization. We indexed salivary biomolecules in 35 whole non-stimulated saliva samples collected in 8 individuals in different days, including organic acids and amino acids and other carbonyl compounds. Among these, 16 whole saliva samples were collected by a single individual over three weeks before, during and after treatment with antibiotic in order to investigate the dynamics of metabolites. The concentrations of the metabolites were compared with the literature data. The multianalyte method here proposed requires a minimal sample handling and it is cost-effectiveness as it makes possible to analyze a high number of samples with basic instrumentation. The identification and quantitation of salivary metabolites may allow the definition of potential biomarkers for non-invasive &ldquo, personal monitoring&rdquo, during drug treatments, work out, or life habits over time.

Biomarkers of oxidative stress are generally measured in blood and its derivatives. However, the invasiveness of blood collection makes the monitoring of such chemicals during exercise not feasible. Saliva analysis is an interesting approach in sport medicine because the collection procedure is easy-to-use and does not require specially-trained personnel. These features guarantee the collection of multiple samples from the same subject in a short span of time, thus allowing the monitoring of the subject before, during and after physical tests, training or competitions. The aim of this work was to evaluate the possibility of following the changes in the concentration of some oxidative stress markers in saliva samples taken over time by athletes under exercise. To this purpose, ketones (i.e. acetone, 2-butanone and 2-pentanone), aldehydes (i.e. propanal, butanal, and hexanal), α,β-unsaturated aldehydes (i.e. acrolein and methacrolein) and di-carbonyls (i.e. glyoxal and methylglyoxal) were derivatized with 2,4-dinitrophenylhydrazine, and determined by ultra-high performance liquid chromatography coupled to diode array detector. Prostaglandin E

The bio-engineering technologies of medical devices through nano-structuring and coating was recently proposed to improve biocompatibility and to reduce microbial adhesion in the prevention of implantable device-related infections. Our aim was to evaluate the ability of new nano-structured and coated materials to prevent the adhesion and biofilm formation, according to the American Standard Test Method ASTM-E2647-13. The materials composition was determined by X-ray Fluorescence and Laser Induced Breakdown Spectroscopy. Silver release was evaluated by Inductively Coupled Plasma Mass Spectrometry analysis. The gene expression levels of the Quorum Sensing Las and Rhl system were evaluated by the &Delta, &Delta, Ct method. The Log bacterial density (Log CFU/cm2) on TiAl6V4 was 4.41 &plusmn, 0.76 and 4.63 &plusmn, 1.01 on TiAl6V4-AgNPs compared to 2.57 &plusmn, 0.70 on CoCr and 2.73 &plusmn, 0.61 on CoCr-AgNPs (P &lt, 0.0001, A.N.O.V.A.- one way test). The silver release was found to be equal to 17.8 &plusmn, 0.2 &micro, g/L after the batch phase and 1.3 &plusmn, 0.1 &micro, g/L during continuous flow. The rhlR gene resulted in a 2.70-fold increased expression in biofilm growth on the silver nanoparticles (AgNPs) coating. In conclusion, CoCr showed a greater ability to reduce microbial adhesion, independently of the AgNPs coating. The silver release resulted in promoting the up-regulation of the Rhl system. Further investigation should be conducted to optimize the effectiveness of the coating.

The role of water and hematite (Fe2O3) on the stability of ovalbumin-based model paint layers was investigated by means of DSC and FTIR. The aim of this research is to improve our understanding on the stability of paint layers based on proteinaceous media, assessing the water content and the pigment presence effects. Pigments may play a fundamental role in determining the structure of proteins in paint layers, thus affecting the possible interactions among proteins and the external environment, including humidity. Previous studies revealed that hematite affects the secondary structure of OVA in paint layers, although no experimental evidence of hematite/OVA covalent bonds has been reported in the literature. In this paper we investigate the synergic effect of water and hematite on OVA structure and stability. DSC analyses coupled with FTIR measures on protein hydration revealed that below 30 % of humidity the amount of water strongly influence the protein structure and stability: the less the water content, the higher the protein stability. Furthermore, our results suggest that a water phase separation occurs in the presence of hematite for which, in water-limiting condition, the hematite’s hydration shell becomes almost negligible if compared to the bulk water available for the protein hydration because of the high protein-water affinity. Accordingly, the protein phase humidity is higher than the sample’s nominal value. Paints at the same overall humidity exhibit different protein hydration state following the pigment/binder ratio, and in turn different resistance to damages throughout aging.

To define the role of spleen stiffness (SS) and liver stiffness (LS) in myelofibrosis and other Philadelphia (Ph)-negative myeloproliferative neoplasms (MPNs), we studied, by ultrasonography (US) and elastography (ES), 70 consecutive patients with myelofibrosis (MF) (no.43), essential thrombocythemia (ET) (no.10), and polycythemia vera (PV) (no.17). Overall, the median SS was not different between patients with MF and PV (p = 0.9), however, both MF and PV groups had significantly higher SS than the ET group (p = 0.011 and p = 0.035, respectively) and healthy controls (p &lt, 0.0001 and p = 0.002, respectively). In patients with MF, SS values above 40 kPa were significantly associated with worse progression-free survival (PFS) (p = 0.012, HR = 3.2). SS also correlated with the extension of bone marrow fibrosis (BMF) (p &lt, 0.0001). SS was higher in advanced fibrotic stages MF-2, MF-3 (W.H.O. criteria) than in pre-fibrotic/early fibrotic stages (MF-0, MF-1) (p &lt, 0.0001) and PFS was significantly different in the two cohorts, with values of 63% and 85%, respectively (p = 0.038, HR = 2.61). LS significantly differed between the patient cohort with MF and healthy controls (p = 0.001), but not between the patient cohorts with ET and PV and healthy controls (p = 0.999 and p = 0.101, respectively). We can conclude that organ stiffness adds valuable information to the clinical work-up of MPNs and could be employed to define patients at a higher risk of progression.

This paper provides a case-study analysis on a thallium contamination related to the past activity in the dismissed mining sites of Monte Arsiccio and Pollone (Lucca Province, Tuscany, Italy). This site has received a lively public attention in recent times, after the finding of thallium at concentration of concern in drinkable waters, far exceeding the U.S. EPA threshold of 2 μg/L. Already published studies, plus original data, focusing on the different aspects of this case study are here reviewed highlighting how past-mine wastes can affect a whole eco-system, potentially causing adverse health effects in the population living in the area via environmental exposure. After a brief introduction on the mining activity in Tuscany (Section 1), the paper focuses on the geochemical processes behind the release of thallium in the area subject of the study (Sections 2–4), the status of its contamination in different ecological compartments (Sections 5–9) and the exposure of the local inhabitants (Section 10). As final remarks, considerations about possible health impacts are presented. The aim is to contribute to the proactive detection of environmental threats mainly related to thallium hazard and past mining activities, in order to prevent negative impacts to the ecosystem and human health, and to contribute in planning mitigation requirements.

We report a novel study based on analytical pyrolysis coupled with mass spectrometry to investigate, at the molecular level, the formation of aggregates and cross-linked structures in ovalbumin (OVA). For this scope, OVA was dissolved in water at different concentrations and temperatures (up to 80 °C), and was added with 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC). The formation of β-sheets and intermolecular aggregates, which are stabilized by weak hydrophobic and hydrogen bonds, is favoured in OVA by higher protein concentration and temperatures. The cross-linker (EDC) gives the formation of covalent bonds randomly distributed in the protein, inducing significant portions of random coil structures in OVA. FTIR-ATR spectroscopy was employed to study the protein conformation. Evolved gas analysis coupled with mass spectrometry (EGA-MS) and pyrolysis coupled with gas chromatography mass spectrometry (Py-GC–MS) were used to characterise the gaseous compounds evolved during pyrolysis at the different temperatures. Aggregation and cross-linking increase the thermal stability of OVA and significantly affect its pyrolytic profile. The study reveals that analytical pyrolysis coupled to mass spectrometry can be used to gain insights into the protein structure.

The high toxicity of cyanide, along with its widespread industrial use, has fuelled interest in the development of analytical methods for its determination in complex matrices. In this study, we propose a novel approach for the measurement of total cyanide in soil samples based on single-step derivatization with pentafluorobenzyl bromide (F₅Bn−Br) followed by quantitation with gas chromatography mass spectrometry in negative chemical ionization mode. The reaction between CN⁻ and F₅Bn−Br resulted in the identification of several derivatives such as F₅Bn−CN, (F₅Bn)(F₅Ph)CH−CN, and (F₅Bn)₂(F₅Ph)C−CN. The relative proportion between such compounds was dependent on experimental conditions. When a 100 μL aliquot of an alkaline-aqueous extract was reacted with 700 μL of 1.3% F₅Bn−Br in acetone, the tri-alkylated derivative was the most abundant. In such conditions a detection limit of 0.5 ng/g of CN⁻ was attained. Soil samples were initially spiked with an alkaline solution of K¹³C¹⁵N internal standard and suspended in 7.5% aqueous NaOH. Determination of total cyanide was achieved by digestion of the alkaline extract with H₃PO₄ to produce HCN which was then trapped in 0.1% NaOH in a sealed double vial system, followed by reaction with F₅Bn−Br. Isotope dilution calibration was chosen for quantitation, and the validity of the novel method was demonstrated by analysis of soil Certified Reference Materials (CRMs) and by spike recovery tests., yes

This work investigates the application of novel sorption materials to heat-powered desalination systems. Two ionic liquids 1-ethyl-3-methylimidazolium acetate (Emim-Ac) and 1-ethyl-3-methylimidazolium methanesulfonate (Emim-Oms) ionic liquids were impregnated in two silica supports, namely Syloid AL-1FP and Syloid 72FP. Emim-Ac and Emim-Oms composite sorbents have been compared on morphology, water vapor sorption equilibrium and heat of sorption. Fourier-transform infrared spectroscopy shows the ionic liquid partly organises on the silica surface. When used in a sorption desalination process powered by low grade heat at 60°C, these composites have exceptionally high theoretical working capacities ranging from 1 to 1.7 gwater gsorbent–1. Experimental tests on a lab scale desalinator show that Emim-Ac/Syloid 72FP in real operating conditions can produce 25 kgwater kgsorbent–1 day–1. To date, this yield is 2.5 times higher than the best achieved with silica gel.

In this work, a straightforward analytical approach based on headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry was developed for the analysis of salivary volatile organic compounds without any prior derivatization step. With a sample volume of 500 ?L, optimal conditions were achieved by allowing the sample to equilibrate for 10 min at 50 °C and then extracting the samples for 10 min at the same temperature, using a carboxen/polydimethylsiloxane fibre. The method allowed the simultaneous identification and quantification of 20 compounds in sample headspace, including short-chain fatty acids and their derivatives which are commonly analysed after analyte derivatization. The proof of applicability of the methodology was performed with a case study regarding the analysis of the dynamics of volatile metabolites in saliva of a single subject undergoing 5-day treatment with rifaximin antibiotic. Non-stimulated saliva samples were collected over 3 weeks from a nominally healthy volunteer before, during, and after antibiotic treatment. The variations of some metabolites, known to be produced by the microbiota and by bacteria that are susceptible to antibiotics, suggest that the study of the dynamics of salivary metabolites can be an excellent indirect method for analysing the gut microbiota. This approach is novel from an analytical standpoint, and it encourages further studies combining saliva metabolite profiles and gut microbiota dynamics. [Figure not available: see fulltext.]

A mini review of the toxicity of Thallium (Tl) at low doses is herein presented. Thallium has severe toxicity. Although its acute biological effects have been widely investigated and are well known, its biological effects on human health and in cell cultures at low doses (

Clove buds is a spice of relevance in food, traditional medicine, pharmaceutics and cosmetics and, among the spices, they have the highest content of total polyphenols with exceptional antiviral and antimicrobial properties. Various approaches have been reported for the isolation of essential oil from clove buds. Nonetheless, the qualitative and quantitative analysis of hydrosoluble polyphenols and solid residues simultaneously yielded during the extraction process has not been explored yet. This work is focused on the analysis of some variables effect on yield and composition of the clove buds essential oils on a green microwave assisted extraction, and the characterization and quantification of the different compounds obtained from the extraction process. A versatile coaxial dipole antenna, to directly apply the electromagnetic energy inside the extraction medium, was used to thermally activate the hydrodistillation. The composition profiles of clove buds essential oil and hydrosoluble polyphenols obtained during in-situ microwave assisted extraction (IMWAE) were analysed and quantified by head space gas chromatography mass spectrometry (HS-GC–MS) and liquid chromatography with UV/visible diode array/fluorescence detector (HPLC-DAD-FD). The solid residue was characterized by Fourier Transform Infrared (FTIR) spectroscopy and its composition in term of lignin, cellulose and hemicellulose was predicted. The green IMWAE process was compared with the conventional hydrodistillation (CH) in terms of yield and quality of isolated products. Thermogravimetry coupled to FTIR analyses of the evolved gases from the solid residue evidenced that the solid residue obtained from IMWAE of clove buds is richer in cellulose-hemicellulose than the residue obtained from CH. This can be because of microwaves that allow to remove a higher amount of phenolic compounds/lignin oligomers. The enthalpy of combustion values (ΔcH) (kJ/g) of IMWAE and CH residues were determined by calorimetric combustion and were compared with the –ΔcH (kJ/g) values calculated using the hemicellulose, cellulose and lignin compositions predicted by partial least square chemometrics. The ΔcH highlighted the energetic features of solid residues from IMWAE and CH for their potential uses as alternative biomass for fuel production and here firstly reported for this kind of biomass. The extraction approach here presented is environmentally friendly, highly flexible, easily controllable, time saving, and enables to break the scale-up barrier in microwave assisted industrial processes aimed to valorise aromatic herbs and eventually to exploit vegetable wasting materials. This leads to a lowering of production costs and, therefore, of the market price of isolated extracts from aromatic herbs.

Superparamagnetic iron oxide nanoparticles (SPIONs) have received increasing interest as contrast media in biomedical imaging and innovative therapeutic tools, in particular for loco-regional ablative treatments and drug delivery. The future of therapeutic applications would strongly benefit from improving the capability of the nanostructured constructs to reach the selected target, in particular beyond the intravascular space. Besides the decoration of SPIONs surface with ad hoc bioactive molecules, external magnetic fields are in principle able to remotely influence SPIONs' physiological biodistribution and concentrate them to a specific anatomical region or portion of a tissue. The reduction of SPIONs administered to the body and the need for defining the effective SPIONs local concentration suggest that PET/CT may be a method to quantitatively detect the nanoparticles accumulation in vivo at low concentration and assess their tridimensional distribution in response to an external magnetic field and in relation to the local anatomy highlighted by CT imaging. Here, we report on the possibility to assess the spatial distribution of magnetically-driven radiolabelled SPIONs in a peripheral tissue (mouse thigh) with microPET/CT imaging. To this aim we labelled SPIONs using 18 F-2-fluoro-2-deoxyglucose as a synthon, by chemoselective oxime formation between its open-chain tautomer and nanoparticle amino-groups, and employed microPET/CT imaging to measure the radiolabelled construct biodistribution in a small animal model, following intravenous administration, with and without the application of a permanent magnet onto the skin. The in vivo and ex vivo results showed that micro-PET/CT was able to demonstrate the localizing action of the magnet on SPIONs and provide information, in a multimodal 3D data set, about SPIONs biodistribution taking into account the local anatomy. Copyright © 2017 John Wiley & Sons, Ltd.

Plant hormones play a crucial role in controlling plant growth and development. These groups of naturally occurring substances trigger physiological processes at very low concentrations, which require sensitive techniques for their quantitation. This study reports on the development of a newly synthesized polymer sorbent for the analysis of indole-3-acetic acid (IAA), which is the most important auxin in plants, from complex raw matrices, such as plant extracts. IAA was determined by high-performance liquid chromatography (HPLC) coupled with fluorescence detection (FD). The polymer developed was able to bind about 94% of IAA with a reproducible manner. The release of IAA in methanol was more than 70% for both of them. Non-specific hydrophobic interactions are, likely, the dominant driving force of the binding between IAA and the polymer. This methodology was applied for the determination of IAA in raw lemon leaves. The detection and quantification limits for IAA in real samples were 0.50 ± 0.08 ng/g and 2.64 ± 0.09 ng/g (n = 3, α = 0.05), respectively. As expected, the IAA concentration in uninfected lemon sample was significantly lower respect to the concentration found in infected sample.

International audience; Biomarkers of oxidative stress are generally measured in blood and its derivatives. However, the invasiveness of blood collection makes the monitoring of such chemicals during exercise not feasible. Saliva analysis is an interesting approach in sport medicine because the collection procedure is easy-to-use and does not require specially-trained personnel. These features guarantee the collection of multiple samples from the same subject in a short span of time, thus allowing the monitoring of the subject before, during and after physical tests, training or competitions. The aim of this work was to evaluate the possibility of following the changes in the concentration of some oxidative stress markers in saliva samples taken over time by athletes under exercise. To this purpose, ketones (i.e. acetone, 2-butanone and 2-pentanone), aldehydes (i.e. propanal, butanal, and hexanal), α,β-unsaturated aldehydes (i.e. acrolein and methacrolein) and di-carbonyls (i.e. glyoxal and methylglyoxal) were derivatized with 2,4-dinitrophenylhydrazine, and determined by ultra-high performance liquid chromatography coupled to diode array detector. Prostaglandin E2, F2/E2-isoprostanes, F2-dihomo-isoprostanes, F4-neuroprostanes, and F2-dihomo-isofuranes were also determined by a reliable analytical procedure that combines micro-extraction by packed sorbent and ultra-high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Overall the validation process showed that the methods have limits of detection in the range of units of ppb for carbonyls and tens to hundreds of ppt for isoprostanes and prostanoids, very good quantitative recoveries (90–110%) and intra- and inter-day precision lower than 15%. The proof of applicability of the proposed analytical approach was investigated by monitoring the selected markers of oxidative stress in ten swimmers performing a VO2max cycle ergo meter test. The results highlighted a clear increase of salivary by-products of oxidative stress during exercise, whereas a sharp decrease, approaching baseline values, of these compounds was observed in the recovery phase. This study opens up a new approach in the evaluation of oxidative stress and its relation to aerobic activity.

The heavy metal thallium is an emerging pollutant among the most potentially toxic species to which human populations are exposed. Its harmful effects on living organisms are well-known at high doses, typical of acute intoxication. Its harmful effects at low doses are by far less known. In a previous paper, we reported a TlCl-induced metabolic shift to lactate and ethanol production in living hippocampal HN9.10e neurons that appeared after a single short exposure (48 h) at low doses (1-100 μg/L). This metabolic shift to lactate and ethanol suggests a marked impairment of cell bioenergetics. In this work, we provide detailed evidence for TlCl-induced changes of neuronal morphology and mitochondrial activity. Confocal microscopy and fluorescent probes were used to qualitatively and quantitatively analyze, at the subcellular level, living HN9.10e neurons during and after TlCl exposure. An early onset mitochondrial dysfunction appeared, associated with signs of cellular deregulation such as neurite shortening, loss of substrate adhesion, and increase of cytoplasmic calcium. The dose-dependent alteration of mitochondrial ROS (mtROS) level and of transmembrane mitochondrial potential (ΔΨm) has been observed also for very low TlCl doses (1 μg/L). The treatment with the ATP synthase inhibitor oligomycin revealed a severe impairment of the mitochondrial function, more significant than that measured by the simple quantification of the tetramethylrhodamine methyl ester (TMRM) fluorescence. These results highlight that mitochondria are a key subcellular target of TlCl neurotoxicity. The transmembrane mitochondrial potential was significantly correlated with the ethanol concentration in cell culture medium ( P < 0.001, r = -0.817), suggesting that ethanol could be potentially used as a biomarker of mitochondrial impairment.

The abandoned mining area of Valdicastello Carducci (Tuscany, Italy) is characterized by the massive presence of thallium in the acid mine drainages and in the valley stream crossing the region. We previously found that Tl(III), generally considered the less stable oxidation state of thallium, is present both in the stream and in tap water distributed in the area, whereas acid mine drainages only contain Tl(I). These findings posed some concern related to the reactivity and dispersion of this toxic element in the environment. Since the valence state of thallium determines its toxicity, distribution and mobility, the study of thallium redox speciation appears crucial to understand its environmental behaviour. In this work, water samples collected from the mine drainages and the contaminated stream were adopted as model to study the distribution of aqueous Tl(I)/Tl(III) as a function of light exposure and solution properties and composition. The influence of three light sources and organic acids was evaluated. Thallium speciation was also assessed in tap water after treatment with common oxidizing agents, and in the rust crust collected from the public waterworks.

The aim of our study was to investigate how denaturing agents commonly used in protein analysis influence the labeling between a reactive molecule and proteins. For this reason, we investigated the labeling of ovalbumin (OVA) as a globular model protein with p-hydroxymercurybenzoate (pHMB) in its native state (phosphate buffer solution) and in different denaturing conditions (8 mol L-1 urea, 3 mol L-1 guanidinium thiocyanate, 6 mol L-1 guanidinium chloride, 0.2% sodium dodecyl sulfate, and 20% methanol). In addition to chemical denaturation, thermal denaturation was also tested. The protein was pre-column simultaneously denatured and derivatized, and the pHMB-labeled denatured OVA complexes were analyzed by size exclusion chromatography (SEC) coupled online with chemical vapor generation-atomic fluorescence spectrometry (CVG-AFS). The number of-SH groups titrated greatly depends on the protein structure in solution. Indeed, we found that, depending on the adopted denaturing conditions, OVA gave different aggregate species that influence the complexation process. The results were compared with those obtained by a common alternative procedure for the titration of -SH groups that employs monobromobimane (mBBr) as tagging molecule and molecular fluorescence spectroscopy as detection technique. We also investigated the labeling kinetics for denatured OVA and pHMB, finding that the 4 thiolic groups of OVA have a very different reactivity toward mercury labeling, in agreement with previous studies. (C) 2015 Elsevier Inc. All rights reserved.