Sorption Characteristics and Chromatographic Separation of 90Y3+ from 90Sr2+ from Aqueous Media by Chelex-100 (Anion Ion Exchange) Packed Column.

There is growing demand for separation of 90Y carrier free from 90Sr coexisting to produce high purity 90Y essential for radiopharmaceutical uses. Thus, in this context the sorption profiles of Y3+ and Sr2+ from aqueous solutions containing diethylenetriaminepenta acetic acid (DTPA), ethylenediaminetetra-acetic acid (EDTA), acetic acid, citric acid, or NaCl onto Chelex-100 (anion ion exchange) solid sorbent were critically studied for developing an efficient and low-cost methodology for selective separation of Y3+ from Sr2+ ions (1.0 × 10-5 M). Batch experiments displayed relative chemical extraction percentage (98 ± 5.4%) of Y3+ from aqueous acetic acid solution onto Chelex-100 (anion ion exchanger), whereas Sr2+ species showed no sorption. Hence, a selective separation of Y3+ from its parent 90Sr2+ has been established based upon percolation of the aqueous solution of Y3+ and Sr2+ ions containing acetic acid at pH 1-2 through Chelex-100 sorbent packed column at a 2 mL min-1 flow rate. Y3+ species were retained quantitatively while Sr2+ ions were not sorbed and passed through the sorbent packed column without extraction. The sorbed Y3+ species were then recovered from the sorbent packed column with HNO3 (1.0 M) at a 1.0 mL min-1 flow rate. A dual extraction mechanism comprising absorption associated to "weak-base anion exchanger" and "solvent extraction" of Y3+ as (YCl6)3- and an extra part for "surface adsorption" of Y3+ by the sorbent is proposed. The established method was validated by measuring the radiochemical (99.2 ± 2 1%), radionuclide purity and retardation factor (Rf = 10.0 ± 0.1 cm) of 90Y3+ recovered in the eluate. Ultimately, the sorbent packed column also presented high stability for reusing 2-3 cycles without drop in its efficiency (±5%) towards Y3+ uptake and relative chemical recovery. A proposed flow sheet describing the analytical procedures for the separation of 90Y3+ from 90Sr2+ using chelating Chelex 100 (anion exchange) packed column is also included.

Enhancing the Conductivity and Dielectric Characteristics of Bismuth Oxyiodide via Activated Carbon Doping.

Activated carbon/BiOI nanocomposites were successfully synthesized through a simplistic method. The produced composites were then characterized using XRD, TEM, SEM-EDX, and XPS. The results showed that BiOI with a tetragonal crystal structure had been formed. The interaction between activated carbon and BiOI was confirmed via all the mentioned tools. The obtained nanocomposites' electrical conductivity, dielectric properties, and Ac impedance were studied at 59 KHz-1.29 MHz. AC and dc conductivities were studied at temperatures between 303 and 573 K within the frequency range of 59 KHz-1.29 MHz. The 10% activated carbon/BiOI nanocomposite possessed dc and AC conductivity values of 5.56 × 10-4 and 2.86 × 10-4 Ω-1.cm-1, respectively, which were higher than BiOI and the other nanocomposites. Every sample exhibited increased electrical conductivity values as the temperature and frequency rose, suggesting that all samples had semiconducting behavior. The loss and dielectric constants (ε' and ε″) also dropped as the frequency increased, leading to higher dielectric loss. The Nyquist plot unraveled single semicircle arcs and a decreased bulk resistance, indicating decreased grain boundary resistance. Consequently, the electrical characteristics of BiOI, 1C/BiOI, 5C/BiOI, and 10C/BiOI implied their applicability as dielectric absorbers, charge-stored capacitors, and high-frequency microwave devices.

Enhanced sensitivity in electrochemical detection of ochratoxin A within food samples using ferrocene- and aptamer-tethered gold nanoparticles on disposable electrodes.

Ensuring food security is crucial for public health, and the presence of mycotoxins, produced by fungi in improperly stored processed or unprocessed food, poses a significant threat. This research introduces a novel approach - a disposable aptasensing platform designed for the detection of ochratoxin A (OTA). The platform employs gold-nanostructured screen-printed carbon electrodes functionalized with a ferrocene derivative, serving as an integrated faradaic transducing system, and an anti-OTA aptamer as a bioreceptor site. Detection relies on the ferrocene electrochemical signal changes induced by the aptamer folding in the presence of the target molecule. Remarkably sensitive, the platform detects OTA within the range of 0.5 to 70 ng mL-1 and a detection limit of 11 pg mL-1. This limit is approximately 200 times below the levels stipulated by the European Commission for agricultural commodities. Notably, the sensing device exhibits efficacy in detecting OTA in complex media, such as roasted coffee beans and wine, without the need for sample pretreatment, yielding accurate recoveries. Furthermore, while label-free electrochemical aptasensors have proliferated, this study addresses a gap in understanding the binding mechanisms of some aptasensors. To enhance the experimental findings, a theoretical study was conducted to underscore the specificity of the anti-OTA aptamer as a donor for OTA detection. The molecular docking technique was employed to unveil the key binding region of the aptamer, providing valuable insights into the aptasensor specificity.

Non-enzymatic electrochemical detection of melamine in dairy products by using CuO decorated carbon nanotubes nanocomposites.

Melamine, a typical nitrogen enriched organic compound exhibiting great potential in the industrial sector, is exploited as an adulterant to inflate protein levels in dairy products, can pose serious threats to humans and therefore necessitates its swift detection and precise quantification at its first exposure. In this investigation, sensitive and reliable sensor probes were fabricated using CuO nanoparticles and its nanocomposites (NCs) with carbon nanotubes (CNTs), carbon black (CB), and graphene oxide (GO) to promptly quantify melamine in dairy products. The optical, morphological, and structural characteristics of the CuO-CNT NCs were achieved using diverse instrumental techniques including UV-visible spectroscopy, transmission electron microscopy, X- ray diffraction, Fourier-transform infrared spectroscopy, and X-ray photoelectron spectroscopy and etc. The fabrication of glassy carbon electrodes (GCE) was accomplished by coating CuO-CNT NCs through a binder (5 % nafion). These sensor probes demonstrated outstanding electrochemical sensor performance with CuO-CNT NCs/Nafion/GCE sensor probe in terms of very low limit of detection (0.27 nM), good linearity range (0.05-0.5 nM), and relatively high sensitivity (93.924 µA µM-1 m-2) for melamine under optimized experimental conditions. Furthermore, the performance of CuO-CNT NCs/Nafion/GCE coated sensor probes was practically validated for the selective melamine detection in the real sample analysis of commercially available milk brands, which revealed significant figures of merit in a very short response time of 10 s. From the results, it was concluded that the current study might be helpful in the development of an efficient commercial sensor based on ultra-sensitive transition metal oxides in the field of health care monitoring, food stuffs in a broader scale as well as food applications.

A novel chitosan-alginate@Fe/Mn mixed oxide nanocomposite for highly efficient removal of Cr (VI) from wastewater: Experiment and adsorption mechanism.

In this study, the synthesis and experimental theoretical evaluation of a new chitosan/alginate/hydrozyapatite nanocomposite doped with Mn2 and Fe2O3 for Cr removal was reported. The physicochemical properties of the obtained materials were analyzed using the following methods: SEM-EDX, XRD, FTIR, XPS, pH drift measurements, and thermal analysis. The adsorption properties were estimated based on equilibrium and adsorption kinetics measurements. The Langmuir, Freundlich and Temkin isotherms were applied to analyze the equilibrium data. The thermodynamic analysis of adsorption isotherms was performed. A number of equations and kinetic models were used to describe the adsorption rate data, including pseudo-first (PFOE) and pseudo-second (PSOE) order kinetic equations. The obtained test results show that the synthesized biomaterial, compared to pure chitosan, is characterized by greater resistance to high temperatures. Moreover, this biomaterial had excellent adsorption properties. For the adsorption of Cr (VI), the equilibrium state was reached after 120 min, and the sorption capacity was 455.9 mg/g. In addition, DFT calculations and NCI analyses were performed to get more light on the adsorption mechanism of Cr (VI) on the prepared biocomposite.

GC/MS and LC-MS Analysis and in-vitro Antioxidant Activity of Essential Oil and Crude Methanol Extract from the Leaves of Acacia Gerrardii Benth. Growing in Saudi Arabia.

In this study, I determined the essential oil (EO) chemical composition and crude methanol extract (ME) phytochemical profile of the leaves of Acacia gerrardii (ACGL), a plant growing in Saudi Arabia. Additionally, I assessed their in vitro antioxidant activity. The gas chromatography-mass spectrometry analysis of the EO revealed a high content of oxygenated monoterpenes (79.86 %), primarily dominated by pulegone (35.11 %), carvacrol (27.36 %), and neo-dihydrocarveol (4.67 %). The ME was analyzed by liquid chromatography-mass spectrometry to determine its qualitative chemical profile. Four organic acids, eleven phenolic compounds, sixteen flavonoids, nine terpenoids (eight triterpenoids and one diterpenoid), and one coumarin were found in the ME of ACGL. This extract was found to be dominated by 5,6,4-trihydroxy-7,3-dimethoxyflavone (39.30 %), acteoside (30.27 %), nevadensin (7.55 %), isoacteoside (3.08 %) and apiin (3.23 %), and hesperidin (2.73 %). The phenolic (TPC=127.70±1.47 mg gallic acid equivalents/g of extract) and flavonoid (TFC=85.48±0.12 mg quercetin equivalents/g of extract) contents of the ME were also assessed. The in vitro antioxidant activities of both the EO and ME were evaluated using DPPH, ABTS, and ferrous ion chelating effect assays. Compared to the positive control (vit. E and Vit. C), and both extracts exhibited excellent activity.

Gold single atom-based aptananozyme as an ultrasensitive and selective colorimetric probe for detection of thrombin and C-reactive protein.

An ultra-efficient biocatalytic peroxidase-like Au-based single-atom nanozyme (Au-SAzymes) has been synthesized from isolated Au atoms on black nitrogen doped carbon (Au-N-C) using a simple complexation-adsorption-pyrolysis method. The atomic structure of AuN4 centers in black carbon was revealed by combined high-resolution transmission electron microscopy/high-angle annular dark-field scanning transmission electron microscopy. The Au-SAzymes showed a remarkable peroxidase activity with 1.7 nM as Michaelis-Menten constant, higher than most previously reported SAzyme activity. Density functional theory and Monte Carlo calculations revealed the adsorption of H2O2 on AuN4 with formation of OH* and O*. Molecular recognition was greatly enhanced via label-free integration of thiol-terminal aptamers on the surface of single Au atoms (Aptamer/Au-SAzyme) to design off-on ultrasensitive aptananozyme-based sensor for detecting thrombin and CRP with 550 pM and 500 pg mL-1 limits of detection, respectively. The Aptamer/Au-SAzyme showed satisfactory accuracy and precision when applied to the serum and plasma of COVID-19 patients. Due to the maximum Au atom utilization, approximately 3636 samples can be run per 1 mg of gold, highlighting the commercialization potential of the developed Aptamer/Au-SAzyme approach.

Dual-state dual emission from precise chemically engineered bi-ligand MOF free from encapsulation and functionalization with self-calibration model for visual detection.

Synthesis of dual-state dual emitting metal-organic frameworks (DSDE-MOFs) is uncommon and challenging. Additionally, DSDE-MOFs can fulfil the expanding need for on-site detection due to their stability and self-reference for a variety of non-analyte variables. In the present work, a novel intrinsic DSDE of chemically engineered bi-ligand Eu-based MOF (UoZ-1) was designed. The prepared UoZ-1 spherical particles were small-sized around 10-12 nm and displayed blue (425 nm) and red fluorescence (620 nm) at both states, dispersed in liquid and in solid state, when excited at 250 nm. A ratiometry platform was developed since the red emission was quenched by the addition of folic acid and the blue emission was almost remained unaffected. In the fluorometric ratiometric-mode, a dynamic linear range was recorded from 10 to 200 µM with LOD about 0.4 µM. Visual-based detection with assistance of smartphone was developed for quantification based on RGB analysis using Color Grab App. In the visual-mode, LOD as small as 2.3 µM was recorded. By utilizing the intrinsic dual-emitting UoZ-1, highly stable, recyclable, sensitive, and selective on-site visual detection of folic acid can be achieved. UoZ-1, a DSDE-MOF with no encapsulation or functionalization requirements, exhibits great potential for diverse applications.

Ionophore-modified polyaniline-based optode for the determination of hydrogen sulfite levels in beverages, wastewater, and soil.

Sulfite is a very important species, affecting human health, plant and animal life, and environmental sustainability. In this study, for the first time, an ionophore-based ion-selective optode was constructed for hydrogen sulfite determination in beverages, such as Birell® and Sprite®, water, and soil samples; instead of normal pH-chromoionophores, polyaniline film was precipitated on a glass slide and used for the transduction of the sensation mechanism. The ionophore-modified polyaniline-based optode incorporated thiourea derivative as an ionophore and tridodecyl methyl ammonium chloride as an ion-exchanger. The optode film was prepared in situ with a modified chemical polymerization method, and it was characterized using atomic force microscopy (AFM), scanning electron microscopy (SEM), and X-ray diffraction (XRD); also, FTIR spectroscopy was performed for the film before and after interaction with hydrogen sulfite for mechanism elucidation. The optode was applied in the hydrogen sulfite concentration range of 10-1 to 10-5 M with a low detection limit of 8.0 × 10-6 M and minimum interference of other interfering species, such as salicylate, iodide, and sulphide. The response mechanism was due to the ion-exchange of hydrogen sulfite with the anion exchanger, followed by the molecular recognition between thiourea ionophore and hydrogen sulfite, with concomitant redox reaction via the protonation of the polyaniline that causes a decrease in absorbance at 685 nm. The optode was applied successfully for the determination of hydrogen sulfite in real beverages, Birell® and Sprite® without any pretreatment steps. Also, it was applied successfully for the environmental monitoring of hydrogen sulfite in real wastewater and soil samples.

Chemical composition, antioxidant and anti-tyrosinase potentials of Acacia cyclops trunk bark using in vitro and in silico approaches.

The purpose of this paper was to evaluate the phytochemical profile of Acacia cyclops trunk bark methanol extract using LC-MS/MS, as well as to assess its antioxidant and anti-tyrosinase activities. Thus, total phenolic and flavonoid contents of the studied extract were established and 19 compounds were detected and quantified. In addition of their antioxidant potential against DPPH and ABTS assays, in vitro and in silico studies were adopted to evaluate tyrosinase inhibitory property of A. cyclops extract. Methanol trunk bark extract showed significant total phenolic content, antioxidant potential in terms of free radical scavenging, as well as an interesting tyrosinase inhibitory action (IC50= 05.12 ± 0.41 µg/mL). The molecular docking analysis and the drug-likeness prediction of the major selected compounds supported the significant anti-tyrosinase activity of the studied extract. The obtained results suggest that A. cyclops extract could be a promising candidate in the treatment of skin hyperpigmentation disorders.

Sub-femtomolar capacitance-based biosensing of kanamycin using screen-printed electrodes coated with redox-active polymeric films.

An ultrasensitive capacitance-based biosensor has been developed capable of detecting the kanamycin (KAN) antibiotic at sub-femtomolar levels. The biosensor was constructed using a potential-pulse-assisted method, allowing for the layer-by-layer deposition of a melanin-like polymeric film (MLPF) on an electrode surface modified with gold nanoparticles (AuNPs). The MLPF was formed through the electrochemical polymerization of dopamine and the specific kanamycin aptamer. By optimizing the operating parameters, we achieved a label-free detection of kanamycin by monitoring the variation of pseudocapacitive properties of the MLPF-modified electrode using electrochemical impedance spectroscopy. The developed biosensor demonstrated a wide linear response ranging from 1 fM to 100 pM, with a remarkable limit of detection of 0.3 fM (S/N = 3) for kanamycin. Furthermore, the biosensor was successfully applied to detect kanamycin in milk samples, exhibiting good recovery. These findings highlight the promising potential of the aptasensor for determination of antibiotic residues and ensuring food safety. In conclusion, our ultrasensitive capacitance-based biosensor provides a reliable and efficient method for detecting trace amounts of kanamycin in dairy products. This technology can contribute to safeguarding consumer health and maintaining high food safety standards.

Highly sensitive capacitance-based nitrite sensing using polydopamine/AuNPs-modified screen-printed carbon electrode.

Regulatory bodies play a crucial role in establishing limits for food additives to ensure food quality and safety of food products, as excessive usage poses risks to consumers. In the context of processed animal-based foodstuffs, nitrite is commonly utilized as a means to slow down bacterial degradation. In this study, we have successfully leveraged the redox activity of an electrochemically deposited polydopamine (pDA) film onto gold nanoparticle (AuNP)-modified screen-printed electrodes (SPCE) to develop a sensitive and versatile methodology for the detection of nitrite using redox capacitance spectroscopy. By exploiting the interaction of the AuNPs/pDA electroactive interface with the target nitrite ions, we observed distinct changes in the redox distribution, subsequently leading to modifications in the associated redox capacitance. This alteration enables the successful detection of nitrite, exhibiting a linear response within the concentration range of 10 to 500 µM, with a limit of detection of 1.98 µM (S/N = 3). Furthermore, we applied the developed sensor to analyze nitrite levels in processed meats, yielding good recoveries. These results demonstrate the potential of our approach as a promising method for routine detection of ions.

Adsorption and Removal of Tetrabromobisphenol A by Adsorption on Functionalized Mesoporous Silica Nanotubes: Isotherms, Kinetics, Thermodynamics, and Optimization via Box-Behnken Design.

In pursuit of environmental safety, a novel and efficient method-dispersive solid-phase extraction based on functionalized mesoporous silica nanotubes (FMSNT nanoadsorbent)-was developed to remove tetrabromobisphenol A (TBBPA) from water samples. Characterization and comprehensive analysis of the FMSNT nanoadsorbent, including maximum adsorption capacity of 815.85 mg g-1 for TBBPA and its water stability, confirmed its potential. Subsequent analysis revealed the impact of multiple factors, for instance pH, concentration, dose, ionic strength, time, and temperature, on the adsorption process. The findings revealed that the adsorption of TBBPA followed the Langmuir and pseudo-second-order kinetics models while primarily driven by hydrogen bond interactions between bromine ions or hydroxyl groups of TBBPA and amino protons around the cavity. The novel FMSNT nanoadsorbent showed high stability and efficiency even after five times of recycling. Moreover, the overall process was identified as chemisorption, endothermic, and spontaneous. Finally, the Box-Behnken design was applied to optimize the results, confirming good reusability even after five cycles.

Facile synthesis and characterization of Fe3O4/analcime nanocomposite for the efficient removal of Cu(II) and Cd(II) ions from aqueous media.

In the water purification field, heavy metal pollution is a problem that causes severe risk aversion. This study aimed to examine the disposal of cadmium and copper ions from aqueous solutions by a novel Fe3O4/analcime nanocomposite. A field emission scanning electron microscope (FE-SEM), Fourier transform infrared spectroscopy (FT-IR), and X-ray diffraction were used to characterize the synthesized products. The FE-SEM images showed that the analcime and Fe3O4 samples consist of polyhedral and quasi-spherical shapes with average diameters of 923.28 and 28.57 nm, respectively. Besides, the Fe3O4/analcime nanocomposite consists of polyhedral and quasi-spherical shapes with average diameters of 1100.00 nm. The greatest uptake capability of the Fe3O4/analcime nanocomposite toward the copper and cadmium ions is 176.68 and 203.67 mg/g, respectively. The pseudo-second-order kinetic model and Langmuir equilibrium isotherm best describe the uptake of copper and cadmium ions using the Fe3O4/analcime nanocomposite. The uptake of copper and cadmium ions using the Fe3O4/analcime nanocomposite is exothermic and chemical in nature.

Effect of hydrophilic/lipophilic balance on the porogenic properties of non-ionic surfactants for monolith preparation and chromatographic separation.

The effect of hydrophilic/lipophilic balance (HLB) of polyoxyethylene ethers of different chain lengths on the microporogenic properties of the Brij surfactants has been studied. The objective of this work is to help better understand the role of each porogen and to set criteria for selecting the proper non-ionic surfactant, based on the HLB value. Seven recipes of different porogen compositions were first prepared and the highest efficiency was achieved using decane/decanol/dodecanol mixture with Brij® 30. Then, four other Brij surfactants covering the entire HLB scale were tested, and the prepared monoliths were characterized by SEM, BET, FT-IR and chromatography. The results showed that increasing the HLB from 9.72 to 18.84 was accompanied by an increase in monolith density and surface areas. The optimum HLB range was found to be 10 to 15. Surfactants of lower HLB formed either nonporous or less efficient columns, while those of higher HLB formed non-permeable columns. Adjusting the HLB was possible by mixing surfactants of different HLB. The prepared monoliths could be used in the isocratic mode with a mobile phase consisting of a mixture of ACN and water (20:80, v/v) at a flow rate of 1.5 µL min-1 to separate five sulfa drugs. The separation results showed that the elution order of the compounds correlated with their lipophilicity, with sulfamerazine (logp = 0.52) being the first to elute, and sulfaquinoxoline (logp=1.70) being the most retained. The asymmetry factors of the separated compounds ranged between 1.18 and 1.25, and the resolution was found to be in the range 2.92-7.80. The prepared monoliths could be also successfully separate a mixture of four different nonsteroidal anti-inflammatory drugs and a mixture of four benzoic acid derivatives. This work assists in optimizing the surfactant-based porogenic mixture to meet the desired porosity, surface area, morphology and chromatographic separation requirements.

In silico selection of an aptamer for the design of aptamer-modified magnetic beads bearing ferrocene co-immobilized label for capacitive detection of acetamiprid.

In silico evaluation of aptamer/target interactions can facilitate the development of efficient biosensor with high specificity and affinity. In this work, we present in silico, i.e. structural similarity, molecular docking and molecular dynamics selection of the aptamer with sufficient binding properties for acetamiprid (ACE), a nicotine-like pesticide, and its use to design aptamer-modified magnetic beads bearing ferrocene co-immobilized label for capacitive detection of ACE. Taking advantages of the aptamer higher stability and binding affinity, the specific properties of magnetic beads and the redox properties of ferrocene moiety, the developed aptasensor showed promising analytical performances for ACE detection, using electrochemical capacitance spectroscopy, with a linear response ranging from 1 fM to 100 pM and a limit of detection of 0.94 fM (S/N = 3). Furthermore, it was successfully applied to detect ACE in fortified tomatoes samples, proving a promising approach for routine detection of pesticide in real agricultural samples.

Chemical Composition, Toxicity and Repellency of Inula graveolens Essential Oils from Roots and Aerial Parts against Stored-Product Beetle Tribolium castaneum (Herbst).

In this work, essential oils extracted from roots and aerial parts of Inula graveolens by hydrodistillation and their fractions obtained by chromatographic simplification were first investigated for their chemical composition by GC/MS and then evaluated for the first time for their repellency and contact toxicity properties against Tribolium castaneumadults. Twenty-eight compounds were identified in roots essential oil (REO), which accounted for 97.9 % of the total oil composition, with modhephen-8-ß-ol (24.7 %), cis-arteannuic alcohol (14.8 %), neryl isovalerate (10.6 %) and thymol isobutyrate (8.5 %) as major constituents. Twenty-two compounds were found in the essential oil from aerial parts (APEO), which accounted for 93.9 % of the total oil, with borneol (28.8 %), caryophylla-4(14),8(15)-dien-6-ol (11.5 %), caryophyllene oxide (10.9 %), τ-cadinol (10.5 %) and bornyl acetate (9.4 %) as main compounds.REO and APEO displayed stronger repellency after 2 h of exposure (80.0 and 90.0 %, respectively) against T. castaneum at the concentration of 0.12 µL/cm2 . After fractionation, fractions R4 and R5 exhibited greater effects (83.3 % and 93.3 %, respectively) than the roots essential oil. Furthermore, the fractions AP2 and AP3 showed higher repellency (93.3 and 96.6 %, respectively) than the aerial parts oil. The LD50 values of oils from roots and aerial parts topically applied were 7.44 % and 4.88 %, respectively. Results from contact toxicity assay showed that fraction R4 was more effective than the roots oil with LD50 value of 6.65 %. These results suggests that essential oils of roots and aerial parts from I. graveolens may be explored as potential natural repellent and contact insecticides against T. castaneum in stored products.

Photocatalytic Activity of Silicon Nanowires Decorated with PbS Nanoparticles Deposited by Pulsed Laser Deposition for Efficient Wastewater Treatment.

The present work aims to study the photocatalytic properties of nanohybrids composed of silicon nanowires (SiNWs) decorated with PbS nanoparticles (NPs). The elaborated material was intended to be utilized in wastewater treatment. The SiNWs were elaborated from the Metal Assisted Chemical Etching route (MACE), while the PbS NPs were deposited at room temperature onto SiNWs using the pulsed laser deposition (PLD) technique. The influence of decorating SiNWs (having different lengths) with PbS-NPs on their structural, morphological, optoelectronic, and photocatalytic properties was scrutinized. PbS/SiNWs nanohybrids exhibited enhanced photocatalytic degradation towards Black Amido (BA) dye for 20 µm SiNWs length and 0.2% of BA volume concentration. These optimized conditions may insinuate that this nanocomposite-like structure is a promising efficient photocatalytic systems contender, cost-effective, and recyclable for organic compound purification from wastewaters.

Design, Microwave-Assisted Synthesis and In Silico Prediction Study of Novel Isoxazole Linked Pyranopyrimidinone Conjugates as New Targets for Searching Potential Anti-SARS-CoV-2 Agents.

A series of novel naphthopyrano[2,3-d]pyrimidin-11(12H)-one containing isoxazole nucleus 4 was synthesized under microwave irradiation and classical conditions in moderate to excellent yields upon 1,3-dipolar cycloaddition reaction using various arylnitrile oxides under copper(I) catalyst. A one-pot, three-component reaction, N-propargylation and Dimroth rearrangement were used as the key steps for the preparation of the dipolarophiles3. The structures of the synthesized compounds were established by 1H NMR, 13C NMR and HRMS-ES means. The present study aims to also predict the theoretical assembly of the COVID-19 protease (SARS-CoV-2 Mpro) and to discover in advance whether this protein can be targeted by the compounds 4a-1 and thus be synthesized. The docking scores of these compounds were compared to those of the co-crystallized native ligand inhibitor (N3) which was used as a reference standard. The results showed that all the synthesized compounds (4a-l) gave interesting binding scores compared to those of N3 inhibitor. It was found that compounds 4a, 4e and 4i achieved greatly similar binding scores and modes of interaction than N3, indicating promising affinity towards SARS-CoV-2 Mpro. On the other hand, the derivatives 4k, 4h and 4j showed binding energy scores (-8.9, -8.5 and -8.4 kcal/mol, respectively) higher than the Mpro N3 inhibitor (-7.0 kcal/mol), revealing, in their turn, a strong interaction with the target protease, although their interactions were not entirely comparable to that of the reference N3.

Trifluoromethylated Flavonoid-Based Isoxazoles as Antidiabetic and Anti-Obesity Agents: Synthesis, In Vitro α-Amylase Inhibitory Activity, Molecular Docking and Structure-Activity Relationship Analysis.

Diabetes mellitus is a major health problem globally. The management of carbohydrate digestion provides an alternative treatment. Flavonoids constitute the largest group of polyphenolic compounds, produced by plants widely consumed as food and/or used for therapeutic purposes. As such, isoxazoles have attracted the attention of medicinal chemists by dint of their considerable bioactivity. Thus, the main goal of this work was to discover new hybrid molecules with properties of both flavonoids and isoxazoles in order to control carbohydrate digestion. Moreover, the trifluoromethyl group is a key entity in drug development, due to its strong lipophilicity and metabolic stability. Therefore, the present work describes the condensation of a previously synthesized trifluoromethylated flavonol with different aryl nitrile oxides, affording 13 hybrid molecules indicated as trifluoromethylated flavonoid-based isoxazoles. The structures of the obtained compounds were deduced from by 1H NMR, 13C NMR, and HRMS analysis. The 15 newly synthesized compounds inhibited the activity of α-amylase with an efficacy ranging from 64.5 ± 0.7% to 94.7 ± 1.2% at a concentration of 50 µM, and with IC50 values of 12.6 ± 0.2 µM-27.6 ± 1.1 µM. The most effective compounds in terms of efficacy and potency were 3b, 3h, 3j, and 3m. Among the new trifluoromethylated flavonoid-based isoxazoles, the compound 3b was the most effective inhibitor of α-amylase activity (PI = 94.7 ± 1.2% at 50 µM), with a potency (IC50 = 12.6 ± 0.2 µM) similar to that of the positive control acarbose (IC50 = 12.4 ± 0.1 µM). The study of the structure-activity relationship based on the molecular docking analysis showed a low binding energy, a correct mode of interaction in the active pocket of the target enzyme, and an ability to interact with the key residues of glycosidic cleavage (GLU-230 and ASP-206), explaining the inhibitory effects of α-amylase established by several derivatives.