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Atmospheric mass loss plays a major role in the evolution of exoplanets. This process is driven by the stellar high-energy irradiation, especially in the first hundreds of millions of years after dissipation of the proto-planetary disk. A major source of uncertainty in modeling atmospheric photoevaporation and photochemistry is due to the lack of direct measurements of the stellar flux at extreme-UV (EUV) wavelengths. Several empirical relationships have been proposed in the past to link EUV fluxes to emission levels in X-rays, but the stellar samples employed for this aim are heterogeneous, and the available scaling laws provide significantly different predictions, especially for very active stars. We present new far-UV and X-ray observations of V1298 Tau with Hubble Space Telescope/Cosmic Origins Spectrograph and XMM-Newton, aimed to determine more accurately the high-energy emission of this solar-mass pre-main-sequence star, which hosts four exoplanets. Spectroscopic data were employed to derive the plasma emission measure distribution versus temperature, from the chromosphere to the corona, and the possible variability of this irradiation on short and year-long timescales, due to magnetic activity. As a side result, we have also measured the chemical abundances of several elements in the outer atmosphere of V1298 Tau. We employ our results as a new benchmark point for the calibration of the X-ray to EUV scaling laws, and hence to predict the time evolution of the irradiation in the EUV band, and its effect on the evaporation of exo-atmospheres.

Food industry produces significant amount of waste that represents a problem for the sector. However, by-products are also promising sources of compounds which may be reused for their nutritional properties. The aim of this work is to exploit wine-making by-products, obtaining an extract by ultrasound-assisted extraction only using water as solvent. The characteristics of spaghetti enriched with grape marc were assessed and compared to control samples. In particular, total phenolic and flavonoids contents, the antioxidant activity, the cooking quality, and the sensory acceptability were evaluated at various steps of pasta production. The enriched spaghetti showed higher total phenolic and flavonoids contents and higher antioxidant activity than the control pasta. In addition, low cooking losses were found. In terms of sensory properties fortified pasta is acceptable as the traditional product, thus demonstrating that it is possible to exploit food waste to better satisfy consumer demand for healthy food products in a more sustainable perspective.

In the present work we analyzed seven globular clusters (GCs) selected from their location in the Galactic bulge and with metallicity values in the range −1.30 ≲ [Fe/H] ≲ −0.50. The aim of this work is first to derive cluster ages assuming single stellar populations and second to identify the stars from first (1G) and second generations (2G) from the main sequence, subgiant, and red giant branches, and to derive their age differences. Based on a combination of UV and optical filters used in this project, we apply the Gaussian mixture models to distinguish the multiple stellar populations. Applying statistical isochrone fitting, we derive self-consistent ages, distances, metallicities, and reddening values for the sample clusters. An average age of 12.3 ± 0.4 Gyr was obtained both using DSED and BaSTI (accounting atomic diffusion effects) isochrones, without a clear distinction between the moderately metal-poor and the more metal-rich bulge clusters, except for NGC 6717 and the inner halo NGC 6362 with ∼13.5 Gyr. We derived a weighted mean age difference between the multiple populations hosted by each GC of 41 ± 170 Myr adopting canonical He abundances; whereas for higher He in 2G stars, this difference reduces to 17 ± 170 Myr, but with individual uncertainties of 500 Myr. [ABSTRACT FROM AUTHOR]

The Bayesian isochrone fitting using the Markov chain Monte Carlo algorithm is applied, to derive the probability distribution of the parameters age, metallicity, reddening, and absolute distance modulus. We introduce the SIRIUS code by means of simulated color–magnitude diagrams (CMDs), including the analysis of multiple stellar populations (MPs). The population tagging is applied from the red giant branch to the bottom of the main sequence. Through sanity checks using synthetic Hubble Space Telescope CMDs of globular clusters we verify the code reliability in the context of simple and MPs. In such tests, the formal uncertainties in age or age difference, metallicity, reddening, and absolute distance modulus can reach 400 Myr, 0.03 dex, 0.01 mag, and 0.03 mag, respectively. We apply the method to analyze NGC 6752, using Dartmouth stellar evolutionary models. Assuming a single stellar population, we derive an age of 13.7 ± 0.5 Gyr and a distance of , with the latter in agreement within 3σ with the inverse Gaia parallax. In the analysis of the MPs, three populations are clearly identified. From the Chromosome Map and UV/Optical two-color diagrams inspection, we found a fraction of stars of 25 ± 5, 46 ± 7, and 29 ± 5 %, for the first, second, and third generations, respectively. These fractions are in good agreement with the literature. An age difference of 500 ± 410 Myr between the first and the third generation is found, with the uncertainty decreasing to 400 Myr when the helium enhancement is taken into account. [ABSTRACT FROM AUTHOR]

Bulge globular clusters (GCs) with metallicities [Fe/H] ≲ −1.0 and blue horizontal branches are candidates to harbor the oldest populations in the Galaxy. Based on the analysis of HST proper-motion-cleaned color–magnitude diagrams in filters F435W and F625W, we determine physical parameters for the old bulge GCs NGC 6522 and NGC 6626 (M28), both with well-defined blue horizontal branches. We compare these results with similar data for the inner halo cluster NGC 6362. These clusters have similar metallicities (−1.3 ≤ [Fe/H] ≤ −1.0) obtained from high-resolution spectroscopy. We derive ages, distance moduli, and reddening values by means of statistical comparisons between observed and synthetic fiducial lines employing likelihood statistics and the Markov chain Monte Carlo method. The synthetic fiducial lines were generated using α-enhanced BaSTI and Dartmouth stellar evolutionary models, adopting both canonical (Y ∼ 0.25) and enhanced (Y ∼ 0.30–0.33) helium abundances. RR Lyrae stars were employed to determine the HB magnitude level, providing an independent indicator to constrain the apparent distance modulus and the helium enhancement. The shape of the observed fiducial line could be compatible with some helium enhancement for NGC 6522 and NGC 6626, but the average magnitudes of RR Lyrae stars tend to rule out this hypothesis. Assuming canonical helium abundances, BaSTI and Dartmouth models indicate that all three clusters are coeval, with ages between ∼12.5 and 13.0 Gyr. The present study also reveals that NGC 6522 has at least two stellar populations, since its CMD shows a significantly wide subgiant branch compatible with 14% ± 2% and 86% ± 5% for first and second generations, respectively. [ABSTRACT FROM AUTHOR]

We present a photometric and spectroscopic study of multiple populations along the asymptotic giant branch (AGB) of the intermediate-metallicity globular clusters (GCs) NGC 2808 and NGC 6121 (M4). Chemical abundances of O, Na, Mg, Al, Si, Ca, Sc, Ti, V, Cr, Fe, Co, Ni, Zn, Y, and Ce in AGB stars from high-resolution FLAMES+UVES@VLT spectra are reported for both clusters. Our spectroscopic results have been combined with multiwavelength photometry from the Hubble Space Telescope UV survey of Galactic GCs and ground-based photometry, as well as proper motions derived by combining stellar positions from ground-based images and Gaia DR1. Our analysis reveals that the AGBs of both clusters host multiple populations with different chemical compositions. In M4, we have identified two main populations of stars with different Na/O content lying on distinct AGBs in the versus and the V versus pseudo-color–magnitude diagrams. In the more massive and complex GC NGC 2808, three groups of stars with different chemical abundances occupy different locations on the so-called “chromosome map” photometric diagram constructed for AGB stars. The spectroscopic + photometric comparison of stellar populations along the AGB and the red giants of this GC suggests that the AGB hosts stellar populations with a range in helium abundances from primordial to high contents of . By contrast, from our data set, there is no evidence for stars with extreme helium abundance () on the AGB, suggesting that the most He-rich stars of NGC 2808 do not reach this phase. [ABSTRACT FROM AUTHOR]

We used data from the Hubble Space Telescope UV Legacy Survey of Galactic Globular Clusters to select the Blue Straggler Star (BSS) population in four intermediate/high density systems (namely NGC 2808, NGC 6388, NGC 6541, and NGC 7078) through a “UV-guided search.” This procedure consists of using the F275W images in each cluster to construct the master list of detected sources, and then force it to the images acquired in the other filters. Such an approach optimizes the detection of relatively hot stars and allows the detection of a complete sample of BSSs even in the central region of high-density clusters, because the light from the bright cool giants, which dominates the optical emission in old stellar systems, is sensibly reduced at UV wavelengths. Our UV-guided selections of BSSs have been compared to the samples obtained in previous, optical-driven surveys, clearly demonstrating the efficiency of the UV approach. In each cluster we also measured the parameter A+, defined as the area enclosed between the cumulative radial distribution of BSSs and that of a reference population, which traces the level of BSS central segregation and the level of dynamical evolution suffered by the system. The values measured for the four clusters studied in this paper nicely fall along the dynamical sequence recently presented for a sample of 25 clusters. [ABSTRACT FROM AUTHOR]

The UV-initiative Hubble Space Telescope Treasury survey of Galactic globular clusters provides a new window into the phenomena that shape the morphological features of the horizontal branch (HB). Using this large and homogeneous catalog of UV and blue photometry, we demonstrate that the HB exhibits discontinuities that are remarkably consistent in color (effective temperature). This consistency is apparent even among some of the most massive clusters hosting multiple distinct sub-populations (such as NGC 2808, ω Cen, and NGC 6715), demonstrating that these phenomena are primarily driven by atmospheric physics that is independent of the underlying population properties. However, inconsistencies arise in the metal-rich clusters NGC 6388 and NGC 6441, where the discontinuity within the blue HB (BHB) distribution shifts ∼1000–2000 K hotter. We demonstrate that this shift is likely due to a large helium enhancement in the BHB stars of these clusters, which in turn affects the surface convection and evolution of such stars. Our survey also increases the number of Galactic globular clusters known to host blue-hook stars (also known as late hot flashers) from 6 to 23 clusters. These clusters are biased toward the bright end of the globular cluster luminosity function, confirming that blue-hook stars tend to form in the most massive clusters with significant self-enrichment. [ABSTRACT FROM AUTHOR]

Volatile organic compounds (VOCs) are continuously emitted into the atmosphere from natural and anthropogenic sources and rapidly spread from the atmosphere to different environments. A large group of VOCs has been included in the class of air pollutants; therefore, their determination and monitoring using reliable and sensitive analytical methods represents a key aspect of health risk assessment. In this work, an untargeted approach is proposed for the evaluation of the exposure to volatile organic compounds of workers in an engine manufacturing plant by GC-MS measurements, coupled with solid-phase microextraction (SPME). The analytical procedure was optimized in terms of SPME fiber, adsorption time, desorption time, and temperature gradient of the chromatographic run. For the microextraction of VOCs, the SPME fibers were exposed to the air in two different zones of the manufacturing factory, i.e., in the mixing painting chamber and the engine painting area. Moreover, the sampling was carried out with the painting system active and running (system on) and with the painting system switched off (system off). Overall, 212 compounds were identified, but only 17 were always present in both zones (mixing painting chamber and engine painting area), regardless of system conditions (on or off). Finally, a semi-quantitative evaluation was performed considering the peak area value of the potentially most toxic compounds by multivariate data analyses., (© 2024. The Author(s).)

Polycyclic aromatic hydrocarbons (PAHs) are environmental contaminants that can be found in various food products, including those intended for infants. Due to their potential health risks, it is crucial to develop sensitive analytical methods for the accurate determination of PAHs in infant foods. This study describes the development and validation of a highly sensitive method for the quantification of European PAH markers, namely benzo[a]pyrene, benzo[a]anthracene, chrysene, and benzo[b]fluoranthene, using gas chromatography-tandem mass spectrometry (GC-MS/MS), in baby food samples. The first step was the optimization of the sample preparation procedure, performed using different methods based on the QuEChERS approach, also testing different extraction solvents. Several factors such as extraction efficiency, selectivity, and recovery were evaluated to choose the most effective procedure for sample preparation. Furthermore, the GC-MS/MS method was optimized, evaluating parameters such as linearity, sensitivity, accuracy, and robustness using spiked infant food samples. The method demonstrated excellent linearities with a correlation coefficient higher than 0.999 over a wide concentration range, and limits of detection and limits of quantification in the range 0.019-0.036 μg/kg and 0.06-0.11 μg/kg, respectively. Extraction recoveries were between 73.1 and 110.7%, with relative standard deviations always lower than 8%. These findings are compliant with the indications of the European Commission (Reg. 836/2011). To assess the applicability of the method to official control activities, a survey was conducted on commercially available infant food products. Four markers were determined in commercial samples belonging to different food categories for infants and young children. The outcome of this monitoring showed that PAH contamination, in all samples, was below the quantification limits. In conclusion, the developed GC-MS/MS method provides a highly sensitive and reliable approach for the determination of PAHs in baby foods. The optimized sample preparation, instrumental parameters, and validation results ensure accurate quantification of 4 PAHs even at trace levels. This method could contribute to the assessment of PAH exposure in infants and it could support regulatory efforts to ensure the safety and quality of infant food products with regular monitoring., Competing Interests: The authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest. The author(s) declared that they were an editorial board member of Frontiers, at the time of submission. This had no impact on the peer review process and the final decision., (Copyright © 2024 Ingegno, Zianni, Della Rovere, Chiappinelli, Nardelli, Casamassima, Calitri, Quinto, Nardiello and Iammarino.)

Background: Gas chromatography is worldwide recognized as one of the most important analytical techniques, due to its high versatility and reliability. The heart of a gas chromatograph is the column, that allows analyte peak separations and, consequently, accurate qualitative and qualitative analyses. New and more efficient columns are always requested to satisfy new and challenging analytical needs., Results: In this work, imidazolium ionic liquids functionalized pillar [5] arenes have been used for the first time as gas chromatographic stationary phases, considering their highly symmetric pillar-shaped architecture with cavities rich in π-electrons. Four imidazolium ionic liquids functionalized pillar [5] arenes have been tested as stationary phases with numerous analytes and isomers. In particular, one of these showed superior performances if compared to commercial columns, enabling challenging isomeric separations of halogenated benzenes, aromatic aldehydes, and aromatic anilines., Significance and Novelty: To our knowledge, this is the first report on the use of the ionic liquid P[n]A as a stationary phase in chromatography, either in GC or liquid chromatography (LC) separations. This work demonstrates the promising potential of ionic liquid P[n]A stationary phases for chromatographic separations., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2024 Elsevier B.V. All rights reserved.)

Opioids such as heroin, fentanyl, raw opium, and morphine have become a serious threat to the world population in the recent past, due to their increasing use and abuse. The detection of these drugs in biological samples is usually carried out by spectroscopic and/or chromatographic techniques, but the need for quick, sensitive, selective, and low-cost new analytical tools has pushed the development of new methods based on selective nanosensors, able to meet these requirements. Modern sensors, which utilize "next-generation" technologies like nanotechnology, have revolutionized drug detection methods, due to easiness of use, their low cost, and their high sensitivity and reliability, allowing the detection of opioids at trace levels in raw, pharmaceutical, and biological samples (e.g . blood, urine, saliva, and other biological fluids). The peculiar characteristics of these sensors not only have allowed on-site analyses (in the field, at the crime scene, etc.) but also they are nowadays replacing the gold standard analytical methods in the laboratory, even if a proper method validation is still required. This paper reviews advances in the field of nanotechnology and nanosensors for the detection of commonly abused opioids both prescribed (i.e. codeine and morphine) and illegal narcotics (i.e. heroin and fentanyl analogues)., (© The Author(s) 2024. Published by OUP on behalf of the Academy of Forensic Science.)

Neptune-sized planets exhibit a wide range of compositions and densities, depending on factors related to their formation and evolution history, such as the distance from their host stars and atmospheric escape processes. They can vary from relatively low-density planets with thick hydrogen-helium atmospheres 1,2 to higher-density planets with a substantial amount of water or a rocky interior with a thinner atmosphere, such as HD 95338 b (ref.  3 ), TOI-849 b (ref.  4 ) and TOI-2196 b (ref.  5 ). The discovery of exoplanets in the hot-Neptune desert 6 , a region close to the host stars with a deficit of Neptune-sized planets, provides insights into the formation and evolution of planetary systems, including the existence of this region itself. Here we show observations of the transiting planet TOI-1853 b, which has a radius of 3.46 ± 0.08 Earth radii and orbits a dwarf star every 1.24 days. This planet has a mass of 73.2 ± 2.7 Earth masses, almost twice that of any other Neptune-sized planet known so far, and a density of 9.7 ± 0.8 grams per cubic centimetre. These values place TOI-1853 b in the middle of the Neptunian desert and imply that heavy elements dominate its mass. The properties of TOI-1853 b present a puzzle for conventional theories of planetary formation and evolution, and could be the result of several proto-planet collisions or the final state of an initially high-eccentricity planet that migrated closer to its parent star., (© 2023. The Author(s), under exclusive licence to Springer Nature Limited.)

The separation of aromatic isomers, in particular xylene isomers, represents a big issue in chemical and petroleum industries, owing to their similar molecular sizes and boiling points. In this work, the investigation ofpillar[6]arene derivative modified by long alkyl chains (P6A-C10) as a stationary phase for high-resolution gas chromatographic (GC) separations of xylene isomers is presented. Pillar[n]arenes are a new class of macrocyclic hosts that can accommodate specific guests due to their highly symmetrical and rigid pillar architectures with π-electron rich cavities. The P6A-C10 column showed high-resolution performance towards xylene isomers, with peculiar advantages if compared with the commercial HP-5, HP-35, DB-17, and PEG-20Mcolumns.A quantum chemistry calculation has been performed, showing a difference in non-covalent interactions with the P6A-C10 pillar framework, which leads to specific selectivity for xylene isomers.Furthermore, the P6A-C10 column exhibited good repeatability., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2023 Elsevier B.V. All rights reserved.)

In this work, the fabrication, synthesis, and characterization of a new stationary phase based on an amphiphilic pillar[6]arene (P6A-C10-2NH 2 ) for gas chromatographic analyses are reported. The gas chromatography (GC) column prepared with P6A-C10-2NH 2 stationary phase exhibited a medium polarity, an efficiency of 3219 plates/m, and unmatched resolving capabilities toward chloroaniline, bromoaniline, iodoaniline, and toluidine isomers. Furthermore, the P6A-C10-2NH 2 column showed excellent repeatability with maximum relative standard deviations equal to 0.02, 0.07, and 2.56% for run-to-run, day-to-day, and column-to-column, respectively, demonstrating a great potential as a new stationary phase in separation science.

In this work, a novel capillary column (C4A-mPEG) with a calixarene-based polymer stationary phase (poly(ethylene glycol) methyl ether-functionalized 4-tert-butylcalix[4]arene) was designed and used for gas chromatographic (GC) separations. The C4A-mPEG capillary column, prepared by the static coating method, showed moderate polarity and a column efficiency of 2332 plates/m, determined by 1-octanol at 120 °C. The separation features of C4A-mPEG stationary phase, resulting from its unique structure and multiple molecular recognition processes with analytes, including π-π, H-bonding, dipole-dipole, and van der Waals interactions, allowed to obtain high-resolution performances for a wide range of compounds and their isomers, especially benzaldehydes, phenols, and anilines. Moreover, compared with 4-tertbutyl calix[4]arene (C4A) and polyethylene glycol (PEG) stationary phases, a higher resolving capability was also observed for the separation of toluidine and xylidine isomers., (© 2022 Wiley-VHCA AG, Zurich, Switzerland.)

The development of new technologies for the separation, selection, and isolation of microparticles such as rare target cells, circulating tumor cells, cancer stem cells, and immune cells has become increasingly important in the last few years. Microparticle separation technologies are usually applied to the analysis of disease-associated cells, but these procedures often face a cell separation problem that is often insufficient for single specific cell analyses. To overcome these limitations, a highly accurate size-based microparticle separation technique, herein called "rotating magnetic chromatography", is proposed in this work. Magnetic nanoparticles, placed in a microfluidic separation channel, are forced to move in well-defined trajectories by an external magnetic field, colliding with microparticles that are in this way separated on the basis of their dimensions with high accuracy and reproducibility. The method was optimized by using fluorescein isothiocyanate-modified polystyrene particles (chosen as a reference standard) and then applied to the analysis of cancer cells like Hep-3B and SK-Hep-1, allowing their fast and high-resolution chromatographic separation as a function of their dimensions. Due to its unmatched sub-micrometer cell separation capabilities, RMC can be considered a break-through technique that can unlock new perspectives in different scientific fields, that is, in medical oncology.

A two-dimensional microscale carbon fiber/active carbon fiber system combined with a quadrupole time of flight high-resolution mass spectrometry (2DμCFs-QTOF-HRMS) system is proposed for the rapid putative identification of polar, medium-polar and weakly polar constituents in complex matrices while strongly mitigating ionic suppression effects. The capabilities of 2DμCFs-QTOF-HRMS have been proven by analysing the composition of Abelmoschus manihot flower extracts, allowing, in a single run, the detection of 41 known substances and the presence of 6 compounds never revealed before in these samples. 2DμCFs-QTOF-HRMS has been compared with traditional HPLC-MS, showing higher versatility and a significant reduction of both analysis time (70 min to 5 min) and solvent consumption (35 mL to 1.5 mL). A comparison with the results obtained by direct flow-injection MS analyses demonstrated that 2DμCFs-QTOF-HRMS leads to a more comprehensive analysis and to improved detection sensitivity. The proposed method can be considered suitable for the rapid and comprehensive analysis of food, environmental and pharmaceutical complex samples. 2DμCFs-QTOF-HRMS can thus be considered a rapid, versatile, reliable, high-throughput and economical technique that allows for the collection of information on polar, semipolar, and weakly polar components in complex matrices.

Benzene derivatives (BDs) constitute a class of environmental pollutants whose exposure poses a grave risk to human health. These compounds rapidly diffuse from the atmosphere to the marine ecosystem: for this reason, their monitoring in seawater is every day more compelling. In this work, nanoconfined liquid phase nanoextraction (NLPNE), a versatile extraction technique recently described, has been for the first time applied to the gas chromatographic mass spectrometry (GC/MS) analysis of BDs in seawater. Ex-situ and in-situ NLPNE procedures have been developed and optimized in terms of extraction capabilities, analysis time, precision, and accuracy. Compared to the traditional extraction procedures, based on solid-phase microextraction (SPME) and liquid-liquid extraction (LLE), the proposed NLPNE methods allowed a rapid on-site analysis of benzene compounds with low solvent consumption, higher enrichment factors, and improved automation grade. Determination coefficients ranging from 0.9929 to 0.9997 were obtained for all BDs in the range 0.10-500 ng mL -1 and 5.00-500 ng mL -1 , for ex-situ and in-situ NLPNE, respectively. Ex-situ and in-situ limits of detection ranged from 0.2 to 7.6 ng mL -1 and 0.04-1.00 ng mL -1 . Our results suggest that NLPNE coupled to GC-MS can be considered a powerful technique for high-throughput analyses of trace compounds in environmental, food and biological samples., (Copyright © 2021 Elsevier B.V. All rights reserved.)

In this study a volatolomic approach is proposed for the characterization of the volatile organic compound (VOC) composition of essential oils (EOs) extracted from common aromatic plants. Five species (Prunus spinosa L., Salvia officinalis L., Eucalyptus globulus L., Melissa officinalis L. and Mentha x piperita L.), particularly widespread in Southern Italy, were selected as recognized sources of natural bioactive compounds with beneficial properties. Hydro distillation and solid-liquid extraction with ethanol at different percentages were used to obtain EOs, and their extraction capabilities were compared analyzing chromatographic profiles obtained by headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography - mass spectrometry (GC-MS). The analytical procedure was optimized in term of SPME fiber, adsorption time and desorption time. GC-MS analyses were performed allowing the profiling of the VOC fingerprint in each plant extract. Experimental data were processed by a statistical multivariate approach (Analysis of Variance and Principal Component Analysis obtained for compounds and chemical classes), confirming that EO aroma profiles were statistically different for each of the selected five plants. The proposed volatolomic approach has proved to be an easy and efficient tool to study the aroma profile, allowing the collection of specific information and opening new perspectives and opportunities for the detection and identification of VOCs in agricultural and ecological applications., Competing Interests: Declaration of Competing Interest The authors report no declarations of interest., (Copyright © 2021 Elsevier B.V. All rights reserved.)

An untargeted shot-gun approach is described for the ultra-high-resolution analysis of fennel proteins by Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) combined with a home-made Matlab search algorithm. The first step of the proposed bioinformatic strategy was the development of a custom-made fennel protein database, starting from the well-known, on-line available, protein NCBI database, under Foeniculum Vulgare organism, consisting of 231 total proteins. Partial and redundant forms of proteins, repeatedly included in the official NCBI database under different codes, were removed. In the final custom-made database, in addition to the 92 fennel specific non-redundant proteins, 10 proteins belonging to recognized allergenic sources associated with spice-mugwort-allergy syndrome (celery, carrot, parsley, birch, and mugwort) were also included. The second step was the in-silico enzymatic digestion, performed on all the 102 proteins, to obtain a theoretical list of m/z dataset of tryptic peptides. The Matlab processing data was the third and crucial step, necessary to search for in-silico mass calculated peptide sequences in the high resolution ICR mass spectra of the digested fennel extract. The final step was based on database searching in Peptide Mass Fingerprint (PMF) mode by using the matched m/z values as input data. The PMF search results confirmed the presence of 70 proteins (61 fennel specific and 9 allergenic proteins) inside the fennel extract., Competing Interests: The authors declare that they have no known competing financial interests or personal relationships which have or could be perceived to have influenced the work reported in this article., (© 2021 The Author(s). Published by Elsevier Inc.)

A rapid shot-gun method by Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) is proposed for the characterization of fennel proteins. After enzymatic digestion with trypsin, few microliters of extract were analyzed by direct infusion in positive ion mode. A custom-made non-redundant fennel-specific proteome database was derived from the well-known NCBI database; additional proteins belonging to recognized allergenic sources (celery, carrot, parsley, birch, and mugwort) were also included in our database, since patients hypersensitive to these plants could also suffer from fennel allergy. The peptide sequence of each protein from that derived list was theoretically sequenced to produce calculated m/z lists of possible m/z ions after tryptic digestions. Then, by using a home-made Matlab algorithm, those lists were matched with the experimental FT-ICR mass spectrum of the fennel peptide mixture. Finally, Peptide Mass Fingerprint searches confirmed the presence of the matched proteins inside the fennel extract with a total of 70 proteins (61 fennel specific and 9 allergenic proteins)., (Copyright © 2020 Elsevier Ltd. All rights reserved.)

L-Glutamate (L-Glu) is a well-known flavour enhancer that is present in several foodstuffs. Although L-Glu is generally recognized as safe, the use in foodstuffs remains controversial and then its fast and accurate monitoring represents an important issue. In this work a sensitive and interference-free disposable amperometric biosensor for glutamate monitoring in foodstuffs was developed. The biosensor was prepared by immobilizing glutamate oxidase through co-crosslinking with bovine serum albumin and glutaraldehyde onto a screen printed disposable platinum electrode modified with a permselective overoxidized polypyrrole film. The enzyme immobilization was optimized by using different experimental procedures. The optimized glutamate biosensor was integrated in a flow injection system and characterized in terms of linearity (0.005-1.0 mM, r 2  = 0.992), limits of detection (1.8 μM) and quantitation (5.4 μM), repeatability (RSD < 3%) and stability of response under operational conditions (up to 50 h, over 400 analysis). The biosensor showed also excellent anti-interference characteristics towards the main electroactive interferents present in food matrices, and this allowed the application to the accurate monitoring of glutamate in different foodstuffs., Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper., (Copyright © 2020 Elsevier B.V. All rights reserved.)

In this study, an enhanced fully automated approach is described for the protein isolation from soy flour samples by two-dimensional liquid chromatography with active modulation interface. The use of two multi-port switching valves is proposed to on-line connect the first to the second dimension column, thus overcoming the problems associated with the re-mixing effects and incompatibility of eluent composition and pH. A 5-cm long C4 analytical column installed in the interface device allows to focus the proteins coming from the first column (size exclusion chromatography), before their selective elution in the second column (reversed-phase). A trap washing step was included in the total workflow, as a desalting step to remove buffer residues from the eluent of the first column and to enhance the chromatographic performances of the second column. The experimental conditions were optimized by analyses of mixed standard solutions of bovine serum albumin, glucose oxidase, immunoglobulin A, thyroglobulin and myoglobin. Then, the optimized 2D-LC method was applied to the protein analysis in extracts of soy flour, known worldwide as one of the major food allergen sources, with the final aim to recovery sufficient protein amounts for the molecular characterization and the assessment of the pattern of allergenic components., (Copyright © 2019 Elsevier B.V. All rights reserved.)

A sensitive and reproducible screening analytical method is here proposed for the determination of six non dioxin-like polychlorinated biphenyls (NDL-PCBs, congener 28, 52, 101, 138, 153, 180) in chicken eggs based on accelerated solvent extraction (ASE) procedure for the fat extraction and determination, a solid phase extraction (SPE) sample clean-up process, and a gas chromatography - electron capture detection (GC-ECD) analysis. The optimized chromatographic separation, in less than 25 min, returned good responses for the six NDL-PCBs in the range of 2.5-60.0 µg L -1 , with correlation coefficients always higher than 0.9995. Instrumental limits of detection were between 0.08-0.35 µg L -1 , corresponding to 0.05 and 0.23   ng g -1 fat in the matrix, while method detection limits, calculated on spiked egg samples, ranged from 1.6 to 3.5   ng g -1 fat. The method has been extensively validated in terms of selectivity, sensitivity, recovery, precision, ruggedness and measurement uncertainty, following the European Directives.

In this work, an automated 2D-LC approach for protein isolation from egg samples on preparative scale is proposed. The method is based on the use of a C18 guard column installed in a switching valve to focus the proteins coming from the first dimension column, before their elution in the second column. For the first dimension separation, a size-exclusion column, packed with 3 μm ultrapure silica particles was used. An RP column based on core-shell technology was used for the second dimension separation. A standard mixture of BSA, β-lactoglobulin, and glucose oxidase, chosen as a protein model system, was used to optimize the chromatographic separation conditions. The fully automated workflow allowed to isolate, in a single-chromatographic analysis, a protein amount of 50 μg for each peak fraction, with a total time of 15 min for the first separation and additional 30 min of the second separation for each trapped protein. The final aim was the development of proper analytical tools for protein isolation from foodstuffs to be used for the molecular identification by MS, as well as for biotherapeutic uses, allergy testing, and large-scale investigations in biological systems., (© 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)