U(VI) adsorption by biochar fiber–MnO2 composites

The removal of U(VI) by biochar fibers from aqueous solutions has been investigated prior and after MnO₂ surface-deposition. The removal efficiency has been studied as a function of pH, U(VI) concentration, ionic strength, temperature and contact time. The fibers morphology and surface complexes were analyzed by SEM–EDX and FTIR, respectively. Evaluation of the experimental data indicates that the composite presents extraordinary adsorption capacity (q_max = 3.8 mmol g⁻¹, 904 mg g⁻¹), which is attributed to the formation of inner-sphere surface complexes, and that the adsorption reaction is a relatively fast, endothermic and entropy-driven process.

     

Elucidating the Structural Composition of an Fe–N–C Catalyst by Nuclear‐ and Electron‐Resonance Techniques

Fe–N–C catalysts are very promising materials for fuel cells and metal–air batteries. This work gives fundamental insights into the structural composition of an Fe–N–C catalyst and highlights the importance of an in‐depth characterization. By nuclear‐ and electron‐resonance techniques, we are able to show that even after mild pyrolysis and acid leaching, the catalyst contains considerable fractions of α‐iron and, surprisingly, iron oxide. Our work makes it questionable to what extent FeN₄ sites can be present in Fe–N–C catalysts prepared by pyrolysis at 900 °C and above. The simulation of the iron partial density of phonon states enables the identification of three FeN₄ species in our catalyst, one of them comprising a sixfold coordination with end‐on bonded oxygen as one of the axial ligands.     

Metric Entropy of Convex Hulls in Banach Spaces

The paper presents diverse methods for estimating the coveringnumber of a precompact subset of a Banach space when the entropyof the set of its extremal points is already known. In the caseof a Hilbert space, the Gelfand diameters of the subset arealso estimated.     

On the entropy of the convex hull of finite sets

We give estimates for the entropy numbers and the Gelfand diameters of the symmetric convex hull of a finite number of points in a Banach or a Hilbert space.

     

Exploring the 2′-Hydroxy-Chalcone Framework for the Development of Dual Antioxidant and Soybean Lipoxygenase Inhibitory Agents

2′-hydroxy-chalcones are naturally occurring compounds with a wide array of bioactivity. In an effort to delineate the structural features that favor antioxidant and lipoxygenase (LOX) inhibitory activity, the design, synthesis, and bioactivity profile of a series of 2′-hydroxy-chalcones bearing diverse substituents on rings A and B, are presented. Among all the synthesized derivatives, chalcone 4b, bearing two hydroxyl substituents on ring B, was found to possess the best combined activity (82.4% DPPH radical scavenging ability, 82.3% inhibition of lipid peroxidation, and satisfactory LOX inhibition value (IC₅₀ = 70 μM). Chalcone 3c, possessing a methoxymethylene substituent on ring A, and three methoxy groups on ring B, exhibited the most promising LOX inhibitory activity (IC₅₀ = 45 μM). A combination of in silico techniques were utilized in an effort to explore the crucial binding characteristics of the most active compound 3c and its analogue 3b, to LOX. A common H-bond interaction pattern, orienting the hydroxyl and carbonyl groups of the aromatic ring A towards Asp768 and Asn128, respectively, was observed. Regarding the analogue 3c, the bulky (-OMOM) group does not seem to participate in a direct binding, but it induces an orientation capable to form H-bonds between the methoxy groups of the aromatic ring B with Trp130 and Gly247.     

Characterization and Differentiation of Fresh Orange Juice Variety Based on Conventional Physicochemical Parameters,Flavonoids, and Volatile Compounds Using Chemometrics

The present study focused on the possibility of differentiating fresh-unprocessed orange juice according to botanical origin (variety), based on the use of conventional physico-chemical parameters, flavonoids, and volatile compounds, in combination with chemometrics. For this purpose, oranges from seven different varieties were collected during the harvest years of 2013–2014 and 2014–2015 from central and southern Greece. The physico-chemical parameters that were determined included: electrical conductivity, acidity, pH, and total soluble solids. The flavonoids: hesperidin, neohespseridin, quercetin, naringin, and naringenin were determined using high-performance liquid chromatography (HPLC-DAD). Finally, volatile compounds were determined using headspace solid-phase micro-extraction in combination with gas chromatography-mass spectrometry (HS-SPME/GC-MS). Statistical treatment of data by multivariate techniques showed that orange juice variety had a significant (p < 0.05) impact on the above analytical parameters. The classification rate for the differentiation of orange juice according to orange variety using multivariate analysis of variance (MANOVA) and linear discriminant analysis (LDA) was 89.3%, based on the cross-validation method.     

Analysis of IV Drugs in the Hospital Workflow by Raman Spectroscopy: The Case of Piperacillin and Tazobactam

Medical errors associated with IV preparation and administration procedures in a hospital workflow can even cost human lives due to the direct effect they have on patients. A large number of such incidents, which have been reported in bibliography up to date, indicate the urgent need for their prevention. This study aims at proposing an analytical methodology for identifying and quantifying IV drugs before their administration, which has the potential to be fully harmonized with clinical practices. More specifically, it reports on the analysis of a piperacillin (PIP) and tazobactam (TAZ) IV formulation, using Raman spectroscopy. The simultaneous analysis of the two APIs in the same formulation was performed in three stages: before reconstitution in the form of powder without removing the substance out of the commercial glass bottle (non-invasively), directly after reconstitution in the same way, and just before administration, either the liquid drug is placed in the infusion set (on-line analysis) or a minimal amount of it is transferred from the IV bag to a Raman optic cell (at-line analysis). Except for the successful identification of the APIs in all cases, their quantification was also achieved through calibration curves with correlation coefficients ranging from 0.953 to 0.999 for PIP and from 0.965 to 0.997 for TAZ. In any case, the whole procedure does not need more than 10 min to be completed. The current methodology, based on Raman spectroscopy, outweighs other spectroscopic (UV/Vis, FT-IR/ATR) or chromatographic (HPLC, UHPLC) protocols, already applied, which are invasive, costly, time-consuming, not environmentally friendly, and require specialized staff and more complex sample preparation procedures, thus exposing the staff to hazardous materials, especially in cases of cytotoxic drugs. Such an approach has the potential to bridge the gap between experimental setup and clinical implementation through exploitation of already developed handheld devices, along with the presence of digital spectral libraries.     

Preparation of Reinforced Anisometric Patchy Supraparticles for Self-Propulsion

The preparation of fumed silica-based anisometric supraparticles with well-defined catalytically active patches suitable for self-propulsion is presented here. These sub-millimeter-sized particles can self-propel as they contain Pt-covered magnetite (Fe₃O₄) nanoparticles, where the Pt can decompose catalytically a “fuel” like H₂O₂ and thereby propel the supraparticles. By their magnetic properties, the catalytically active nanoparticles can be concentrated in patches on the supraparticle surface. The goal is to obtain robust supraparticles with well-defined patchiness and long-time stability during self-propulsion through evaporation-induced self-assembly (EISA) on a superhydrophobic surface. The latter is a major issue as oxygen evolution can lead to the disintegration of the supraparticles. Therefore, enhanced mechanical stability is sought using a number of different additives, where the best results are obtained by incorporating polystyrene microspheres followed by heat treatment or reinforcement with microfibrillated cellulose (MFC) and sodium trisilicate (Na₂SiO₃). The detailed internal structure of the different types of particles is investigated by confocal micro-X-ray fluorescence spectroscopy (CMXRF), which allows for precisely locating the catalytic Fe₃O₄@Pt nanoparticles within the supraparticles with a resolution in the µm range. The insights on the supraparticle structure, together with their long-time stability, allow fabricating optimized patchy supraparticles for potential applications in propulsion-enhanced catalysis.