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    Acetamiprid's degradation products and mechanism: Part II – Inert atmosphere and charge storage

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    Reuse and/or recycling of spent adsorbents is taking a central role in modern thinking and catalyzed carbonization is the way forward. Herein we explore the carbonization of adsorbed acetamiprid, in an inert atmosphere, as a way of recycling and producing nitrogen-rich carbon material for potential use in supercapacitors. Added value material and the reuse of the adsorbent were achieved by carbonization at 700 °C under argon. The formation of a nitrogen-doped carbon layer as an active material on the adsorbent, bonded through a C-Si linkage, has been conclusively verified through elemental composition quantification using XPS and EDX measurements. Two-stage catalytic decomposition and condensation of the adsorbed pesticide is followed by TGA and TPD-MS. Attained carbon-based materials give stable Faradaic capacitance with a slight dependency on the number of adsorbing cycles. Capacitance calculated with respect to the adlayer carbon material reaches values as high as 610 F g−1. Galvanostatic Charge/Discharge measurement confirmed the stability of explored materials with a slight increase in capacitance over 1000 cycles. The presented results envisage electroactive materials preparation from environmental pollutants, adding value to spent adsorbents

    Preparation of cyclopropanone 2,2,2-trifluoroethoxy hemiacetals via oxyallyl cation

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    Hemiacetals of cyclopropanone can be isolated and stocked, contrary to their highly reactive parent ketone. However, they are not readily converted to cyclopropanone, which limits their use as its synthetic equivalents. 2,2,2-trifluoroethoxy hemiacetals are expected to be better cyclopropanone surrogates, however, they have never been prepared, so far. We show that oxyallyl cations with a heteroatom in the -position can be intercepted with 2,2,2-trifluoroethanol, with formation of cyclopropanone trifluoroethoxy hemiacetals stable enough to be isolated, purified and characterized. These species can serve as synthetic equivalents of cyclopropanone under mild conditions.Dedicated to Professor Samir Zard, with admiration for his outstanding scientific achievements

    Silver(I) complexes containing antifungal azoles: significant improvement of the anti-Candida potential of the azole drug after its coordination to the silver(I) ion

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    Inspired by the emergence of resistance to currently available antifungal therapy and by the great potential of metal complexes for the treatment of various diseases, we synthesized three new silver(I) complexes containing clinically used antifungal azoles as ligands, [Ag(ecz)2]SbF6 (1, ecz is econazole), {[Ag(vcz)2]SbF6}n (2, vcz is voriconazole), and [Ag(ctz)2]SbF6 (3, ctz is clotrimazole), and investigated their antimicrobial properties. The synthesized complexes were characterized by mass spectrometry, IR, UV-vis and 1H NMR spectroscopy, cyclic voltammetry, and single-crystal X-ray diffraction analysis. In the mononuclear complexes 1 and 3 with ecz and ctz, respectively, the silver(I) ion has the expected linear geometry, in which the azoles are monodentately coordinated to this metal center through the N3 imidazole nitrogen atom. In contrast, the vcz-containing complex 2 has a polymeric structure in the solid state in which the silver(I) ions are coordinated by four nitrogen atoms in a distorted tetrahedral geometry. DFT calculations were done to predict the most favorable structures of the studied complexes in DMSO solution. All the studied silver(I) complexes have shown excellent antifungal and good to moderate antibacterial activities with minimal inhibitory concentration (MIC) values in the ranges of 0.01–27.1 and 2.61–47.9 μM on the selected panel of fungi and bacteria, respectively. Importantly, the complexes 1–3 have exhibited a significantly improved antifungal activity compared to the free azoles, with the most pronounced effect observed in the case of complex 2 compared to the parent vcz against Candida glabrata with an increase of activity by five orders of magnitude. Moreover, the silver(I)-azole complexes 2 and 3 significantly inhibited the formation of C. albicans hyphae and biofilms at the subinhibitory concentration of 50% MIC. To investigate the impact of the complex 3 more thoroughly on Candida pathogenesis, its effect on the adherence of C. albicans to A549 cells (human adenocarcinoma alveolar basal epithelial cells), as an initial step of the invasion of host cells, was studied

    Investigation of the Potential of Selected Food-Derived Antioxidants to Bind and Stabilise the Bioactive Blue Protein C-Phycocyanin from Cyanobacteria Spirulina

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    Blue C-phycocyanin (C-PC), the major Spirulina protein with innumerable health-promoting benefits, is an attractive colourant and food supplement. A crucial obstacle to its more extensive use is its relatively low stability. This study aimed to screen various food-derived ligands for their ability to bind and stabilise C-PC, utilising spectroscopic techniques and molecular docking. Among twelve examined ligands, the protein fluorescence quenching revealed that only quercetin, coenzyme Q10 and resveratrol had a moderate affinity to C-PC (Ka of 2.2 to 3.7 × 105 M–1). Docking revealed these three ligands bind more strongly to the C-PC hexamer than the trimer, with the binding sites located at the interface of two (αβ)3 trimers. UV/VIS absorption spectroscopy demonstrated the changes in the C-PC absorption spectra in a complex with quercetin and resveratrol compared to the spectra of free protein and ligands. Selected ligands did not affect the secondary structure content, but they induced changes in the tertiary protein structure in the CD study. A fluorescence-based thermal stability assay demonstrated quercetin and coenzyme Q10 increased the C-PC melting point by nearly 5 °C. Our study identified food-derived ligands that interact with C-PC and improve its thermal stability, indicating their potential as stabilising agents for C-PC in the food industry

    Nano-size cobalt-doped cerium oxide particles embedded into graphitic carbon nitride for enhanced electrochemical sensing of insecticide fenitrothion in environmental samples: An experimental study with the theoretical elucidation of redox events

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    In the present work, a nanocomposite, based on embedding Co-doped CeO2 nanoparticles into graphitic carbon nitride (g-C3N4), was applied to functionalize commercial glassy carbon paste. This is the first application of the electrochemical sensor, developed through the proposed procedure, in electrochemical sensing. The sensor was utilized for the electrochemical determination of organophosphate pesticide fenitrothion (FNT). Cyclic voltammetry identified reversible oxidation of FNT (oxidation at 0.18 V and reduction at 0.13 V) and additional reduction at 0.62 V vs. Ag/AgCl in HCl solution (pH =1). Theoretical calculations were carried out to model and elucidate experimentally observed redox processes. Special attention was devoted to modeling experimental conditions, and based on the obtained results, a detailed redox mechanism of the investigated analyte was proposed. This represents the first complete and unambiguous elucidation of the FNT redox mechanism, supported by joined experimental and theoretical data. Square wave voltammetry (SWV) was utilized for quantification, whereby the FNT oxidation peak was chosen for monitoring the analyte concentration. The developed sensor provided a nanomolar detection limit (3.2 nmol L 1), a wide linear concentration range (from 0.01 to 13.7 μmol L 1), and good precision, repeatability, and selectivity towards FNT. Practical application possibility was explored by testing the sensor performance for examining tap water and apple samples. Recovery tests, conducted during the FNT-spiked sample assays, showed a great application capability of the developed sensor for real-time monitoring of FNT traces in environmental samples

    Assessment of the ecological status of large lowland rivers (Sava and Tisa, Serbia) based on digital microscopic investigation of the diatom communities

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    Large lowland rivers represent an important type of ecosystem that has been under a constant anthropogenic influence (industry, thermal power plants, untreated communal water, and agriculture) for centuries, which has led to most of them no longer meeting natural reference conditions. These pressures affect diatom communities which represent a reliable bioindicator of the overall degradation of water bodies. The current study provides detailed information about benthic diatoms from the large international lowland rivers Sava and Tisa, analyzed using digital microscopy. Using the digital method and the BIIGLE 2.0 image annotation system, a total of 205 and 206 diatom taxa in the Sava and Tisa rivers were identified, belonging to 65 and 63 genera, respectively. Some of the dominant genera in the Sava River were Achnanthidium, Cocconeis, Gyrosigma, and Navicula, while in the Tisa River, mostly centric diatoms (Discostella, Cyclotella, Stephanodiscus) were dominant. Most of the recorded species are alkaliphilic and characteristic of running waters with high trophic conditions. The presence of halophilic taxa was also noted (e.g. Bacillaria paxilifera, Tryblionella species, Nitzschia clausii, Navicula salinarum). These taxa are sensitive indicators of even short-term changes in lowland lotic ecosystems characterized by elevated conductivity. The diatom indices showed very consistent ecological status, mainly moderate in terms of the general pollution index IPS, and poor to bad ecological status according to trophic diatom indices (Rott TI and TDI)

    Clinopodium L. Taxa from the Balkans - Are There Unique Leaf Micromorphological and Phytochemical Patterns?

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    The concept of the genus Clinopodium L. has changed considerably since its first description. Most of the currently accepted species of the genus have traditionally been treated as separate genera in the group Satureja sensu lato: Clinopodium L., Calamintha sensu Miller or Moench, and Acinos sensu Miller or Moench. This study aimed to gain a better insight into the species diversity of Clinopodium L. from the Balkans by analyzing the taxa that have traditionally been placed in separate genera. The alkane profile and the micromorphological characteristics of the leaves are analyzed. The leaves are visualized using scanning electron microscopy, and alkanes are isolated using n-hexane as a solvent and analyzed using gas chromatography/mass spectrometry. The alkane profile showed the differentiation of the Acinos-group from the other taxa based on the dominant n-C31, while most of the other taxa contained n-C33 as the dominant alkane. The micromorphological features also showed clear differences between the previously recognized genera, especially in the capitate trichomes. The results showed that micromorphological patterns are highly variable in certain groups of the genus Clinopodium

    Bioprospecting of Selected Species of Polypore Fungi from the Western Balkans

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    Growing mushrooms means meeting challenges while aiming for sustainability and circularity. Wherever the producer is located, commercial strains are the same originating from several producers. Customized strains adapted to local conditions are urgently needed. Before introducing new species to the strain development pipeline, the chemical characterization and biological activity of wild ones need to be assessed. Accordingly, the mycoceutical potential of five polypore mushroom species from Serbia was evaluated including: secondary metabolite composition, oxidative damage prevention, anti-tyrosinase, and anti-angiotensin converting enzyme (ACE). The phenolic pattern was comparable in all samples, but the amounts of specific chemicals varied. Hydroxybenzoic acids were the primary components. All samples had varying quantities of ascorbic acid, carotene, and lycopene, and showed a pronounced inhibition of lipid peroxidation (LPx) and ability to scavenge HO•. Extracts were more potent tyrosinase inhibitors but unsuccessful when faced with ACE. Fomitopsis pinicola had the strongest anti-tumor efficacy while Ganoderma lucidum demonstrated strong selectivity in anti-tumor effect in comparison to normal cells. The evaluated species provided a solid foundation for commercial development while keeping local ecology in mind

    The control of morphology and structure of galvanostatically produced tin dendrites by analysis of chronopotentiometry response

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    The influence of chronopotentiometry response on the morphology and structure of galvanostatically synthesized tin dendritic particles has been investigated. Sn dendrites were electrodeposited at the current density 1.5 times larger than the limiting diffusion current density (− 3 mA cm− 2) with various amounts of the electricity (200 and 400 mC), and the obtained morphology and structure of the particles were characterized by SEM and XRD techniques, respectively. The strong effect of the amount of spent electricity on the morphology and structure of the particles was observed, and it is explained by morphological and structural analysis of Sn particles produced potentiostatically at various cathodic potentials selected to be in line with the recorded chronopotentiometry response. The strong correlation among chronopotentiometry response, morphology, and structure of the Sn dendrites was established. The spear-like and the dendrites with prismatic branches possessed the strong (200),(400) preferred orientation, and they were obtained with a chronopotentiometry response of about − 1200 mV vs. Ag/ AgCl. The chronopotentiometry responses in the − 1210 ÷ − 1740 mV vs. Ag/AgCl range caused a formation of the fern-like dendrites with the strong (220),(440) preferred orientation. Based on the obtained results, it follows that the chronopotentiometry analysis represents good diagnostic criteria for obtaining Sn powder particles of desired morphology and structure

    Quality of explosively welded steel plates using demex explosive

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    Заваривање експлозивом се често користи када конвенционалне методе заваривања не могу да обезбеде заварени спој два различита материјала, али и када треба заварити неку специфичну геометрију или велике површине металних плоча. Остваривање споја код заваривања експлозивом се заснива на динамичком дејству великог притиска створеног екплозијом. У ту сврху најчешће се користе индустријски експлозиви ниских параметара детонације, а један од њих је DEMEX, произвођача TRAYAL, из Србије. У овом истраживању DEMEX је примењен за заваривање плоча две различите врсте челика. Пре експерименталног поступка заваривања одабраних металних плоча, експлозив добијен од произвођача је подвргнут улазној контроли квалитета: мерењу његове насипне густине и брзине детонације, коришћењем оптичких сонди и фотодетектора повезаног са електронским бројачем. Експериментална поставка за заваривање била је следећа: експлозив DEMEX у прашкастом стању нанесен је у равномерном слоју преко горње челичне плоче, која је хоризонтално постављена преко доње плоче од друге врсте челика, у паралелном положају, са малим дрвеним дистанцерима ивично постављеним између њих. Активација је извршена електродетонирајућом капислом и малим бустером од пластичног експлозива. Заварени спој је испитан применом метода ултразвучне дефектоскопије, течним пенетрантима и микроструктурне анализе завареног споја. Микроструктурне анализе попречног пресека заварених плоча урађене су на стерео и оптичом микроскопу како би се анализирала зона завареног споја.Explosion welding is often used when conventional welding methods cannot provide welded joint of two dissimilar materials, but also when some specific geometry should be welded, or large surfaces of metal plates. The formation of a joint in explosive welding is based on the dynamic effect of the high pressure created by the explosion. For this purpose, most often some industrial explosives of low detonation parameters are used, and one of them is DEMEX, produced by TRAYAL, Serbia. In this research DEMEX was applied to weld plates of two different types of steel. Prior to the experimental procedure of welding, the selected metal plates, the explosive obtained from the producer was subjected to initial quality control: measurement of its bulk density and detonation velocity, using optical probes and a photodetector connected with an electronic counter. The experimental setup for welding was as follows: explosive DEMEX in powdery state was applied in a uniform layer over the upper plate, which was horizontally placed over the lower plate, in parallel position, with small wooden spacers, marginally placed between them. Activation was performed by an electro-detonating cap and a small booster of plastic explosive. The welded joint was examined using methods of ultrasonic defectoscopy, liquid penetrants testing and microstructural analysis of the welded joint. Cross-sectional microstructural analyses of the welded plates were performed using a stereo and optical microscope to analyze the weld zone


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