Multi-step Synthesis, Characterization and Photophysical Investigation of Novel Biologically Active Heterocyclic Chalcone (AECO).

Novel alkylated heterocyclic chalcone (E)-1-(2-(allyloxy)phenyl)-3-(9-ethyl-9H-carbazol-3-yl)prop-2-en-1-one (AECO) with extended π-bond was prepared by the multi-steps synthesis. The structure of the AECO was established by the spectroscopic technics and purity of the compound was confirmed by the elemental analysis. Physicochemical parameters of the AECO such as molar absorption coefficient, transition dipole moments, stokes shift, oscillator strength and fluorescence quantum yield were calculated in ten various solvents on the basis of polarity of the solvents to see the effect of the solvent with AECO. Interaction of the AECO chromophore with cationic CTAB and anionic SDS surfactants were determined by using the fluorescence spectroscopy techniques. The intensity of the florescence spectrum increase with increasing the concentrations of surfactants. This suggests that strong interaction occurs between AECO with surfactants and this interaction arise from electrostatic forces. So, AECO chromophore could be used as analysis to define the Critical Micelle Concentration (CMC) of the surfactants. In addition the in-vitro antibacterial active of novel heterocyclic chalcone agents four bacteria's strain were evaluated and result showed AECO is beater antibacterial agent against Gram-Negative Bacteria (E. coli and S. flexneri) as compare to the Gram Negative Bacteria with respected to the standard drug Tetracycline.

Hierarchical Tubular Architecture Constructed by Vertically Aligned CoS2 -MoS2 Nanosheets for Hydrogen Evolution Electrocatalysis.

Developing efficient electrocatalysts for the hydrogen evolution reaction (HER) is crucial for establishing a sustainable and environmentally friendly energy system, but it is still a challenging issue. Herein, hierarchical tubular-structured CoS2 -MoS2 /C as efficient electrocatalysts are fabricated through a unique metal-organic framework (MOF) mediated self-sacrificial templating. Core-shell structured MoO3 @ZIF-67 nanorods are used both as a precursor and a sacrificial template to form the one-dimensional tubular heterostructure where vertically aligned two-dimensional CoS2 -MoS2 nanosheets are formed on the MOF-derived carbon tube. Trace amounts of noble metals (Pd, Rh, and Ru) are successfully introduced to enhance the electrocatalytic property of the CoS2 -MoS2 /C nanocomposites. The as-synthesized hierarchical tubular heterostructures exhibit excellent HER catalytic performance owing to the merits of the hierarchical hollow architecture with abundantly exposed edges and the uniformly dispersed active sites. Impressively, the optimal Pd-CoS2 -MoS2 /C-600 catalyst delivers a current density of 10 mA cm-2 at a low overpotential of 144 mV and a small Tafel slope of 59.9 mV/dec in 0.5 m H2 SO4 . Overall, this MOF-mediated strategy can be extended to the rational design and synthesis of other hollow heterogeneous catalysts for scalable hydrogen generation.

Synthesis, photophysical properties, and density functional theory studies of phenothiazine festooned vinylcyclohexenyl-malononitrile.

A novel phenothiazine derivative conjugated with vinylcyclohexenyl-malononitrile (PTZ-CDN) was synthesized through the Knoevenagel reaction of 10-octyl-10H-phenothiazine-3,7-dicarbaldehyde with 2-(3,5,5-trimethylcyclohex-2-en-1-ylidene)-malononitrile and fully characterized. The UV-vis absorption spectra of PTZ-CDN in different solvents showed a λmax band at 497-531 nm with a high molar extinction coefficient attributed to intramolecular charge transfer (ICT) with the characteristics of a π-π* transition. Increasing the solvent polarity resulted in a bathochromic shift of λmax . The PTZ-CDN fluorescence emission spectra were more sensitive to increasing the solvent polarity than the absorption spectra; they displayed a blue shift of λem by 85 nm. To understand the behaviour of the PTZ-CDN derivative, Stokes' shift ( Δ ν ¯ ) with respect to the solvent polarity, Lippert-Mataga and linear solvation-energy relationship (LSER) models were applied in which the LSER showed better regression than the Lippert-Mataga plots (r2 = 0.9627). Finally, the TD-density functional theory (DFT) electronic transition spectra in dioxane and dimethyl formamide (DMF) were calculated. The DFT data showed that λmax resulted from the support of the highest occupied molecular orbital to the lowest unoccupied molecular orbital transition with 74% and 99% in dioxane and DMF, respectively.

Facile Synthesis of Magnetic Nigella Sativa Seeds: Advances on Nano-Formulation Approaches for Delivering Antioxidants and Their Antifungal Activity against Candida albicans.

This article reports on incorporating magnetic nanoparticles into natural carbon frameworks derived from Nigella Sativa seeds and their synthesis via co-precipitation reactions for application in biomedicine. The magnetic Nigella Sativa Seeds (Magnetic NSS), a metal oxide-based bio-nanomaterial, has shown excellent water diaper presence due to the presence of a wide range of oxygenous hydroxyl and carboxyl groups. The physicochemical properties of the composites were characterized extensively using Fourier transform infrared spectroscopy (FTIR), powder-X-ray diffraction (XRD), scanning electron microscopy (SEM), elemental analysis, transmission electron microscopy (TEM), and vibrating-sample magnetometer. Furthermore, synthesized magnetic NSS showed antioxidant and antifungal activity. The antifungal susceptibility was further tested against Candida albicans with a MIC value of 3.125 µg/mL. Analysis of antioxidant defense enzymes was determined quantitatively; the results suggested that antioxidant enzyme activity increase with increased magnetic NSS concentration. Furthermore, biofilm inhibition assay from scanning electron microscopy results revealed that magnetic NSS at the concentration of 3.5 µg/mL has anti-biofilm properties and can disrupt membrane integrity.

Polyphenol-Capped Biogenic Synthesis of Noble Metallic Silver Nanoparticles for Antifungal Activity against Candida auris.

In terms of reduced toxicity, the biologically inspired green synthesis of nanoparticles has emerged as a promising alternative to chemically fabricated nanoparticles. The use of a highly stable, biocompatible, and environmentally friendly aqueous extract of Cynara cardunculus as a reducing and capping agent in this study demonstrated the possibility of green manufacturing of silver nanoparticles (CC-AgNPs). UV-visible spectroscopy validated the development of CC-AgNPs, indicating the surface plasmon resonance (SPR) λmax band at 438 nm. The band gap of CC-AgNPs was found to be 2.26 eV. SEM and TEM analysis examined the surface morphology of CC-AgNPs, and micrographs revealed that the nanoparticles were spherical. The crystallinity, crystallite size, and phase purity of as-prepared nanoparticles were confirmed using XRD analysis, and it was confirmed that the CC-AgNPs were a face-centered cubic (fcc) crystalline-structured material. Furthermore, the role of active functional groups involved in the reduction and surface capping of CC-AgNPs was revealed using the Fourier transform infrared (FTIR) spectroscopic technique. CC-AgNPs were mostly spherical and monodispersed, with an average size of 26.89 nm, and were shown to be stable for a longer period without any noticeable change at room temperature. Further, we checked the antifungal mechanism of CC-AgNPs against C. auris MRL6057. The minimum inhibitory concentrations (MIC) and minimum fungicidal concentrations (MFC) were 50.0 µg/mL and 100.0 µg/mL respectively. The cell count and viability assay confirmed the fungicidal potential of CC-AgNPs. Further, the analysis showed that CC-AgNPs could induce apoptosis and G2/M phase cell cycle arrest in C. auris MRL6057. Our results also suggest that the CC-AgNPs were responsible for the induction of mitochondrial toxicity. TUNEL assay results revealed that higher concentrations of CC-AgNPs could cause DNA fragmentation. Therefore, the present study suggested that CC-AgNPs hold the capacity for antifungal drug development against C. auris infections.

N-doped carbon nanotubes supported CoSe2 nanoparticles: A highly efficient and stable catalyst for H2O2 electrosynthesis in acidic media.

Electrocatalytic oxygen reduction reaction (ORR) provides an attractive alternative to anthraquinone process for H2O2 synthesis. Rational design of earth-abundant electrocatalysts for H2O2 synthesis via a two-electron ORR process in acids is attractive but still very challenging. In this work, we report that nitrogen-doped carbon nanotubes as a multi-functional support for CoSe2 nanoparticles not only keep CoSe2 nanoparticles well dispersed but alter the crystal structure, which in turn improves the overall catalytic behaviors and thereby renders high O2-to-H2O2 conversion efficiency. In 0.1 M HClO4, such CoSe2@NCNTs hybrid delivers a high H2O2 selectivity of 93.2% and a large H2O2 yield rate of 172 ppm·h-1 with excellent durability up to 24 h. Moreover, CoSe2@NCNTs performs effectively for organic dye degradation via electro-Fenton process. Electronic Supplementary Material: Supplementary material (SEM images, EDX mapping images, XPS spectrum, XRD patterns, RRDE voltammogram, Tafel plots, cyclic voltammograms, UV-Vis spectra, and Tables S1) is available in the online version of this article at 10.1007/s12274-021-3474-0.

Bi nanodendrites for efficient electrocatalytic N2 fixation to NH3 under ambient conditions.

Electrochemical N2 reduction has emerged as a sustainable and eco-friendly route for the artificial synthesis of NH3 under ambient conditions, but active electrocatalysts are needed to drive the N2 reduction reaction (NRR). Here, Bi nanodendrites are reported as an efficient NRR electrocatalyst for N2 to NH3 conversion with excellent selectivity. In 0.1 M HCl, this catalyst achieves a large NH3 yield of 25.86 µg h-1 mg-1cat. and a high faradaic efficiency of 10.8% at -0.60 V and -0.55 V versus a reversible hydrogen electrode, respectively, with high electrochemical durability.

Bioinspired Electrocatalyst for Electrochemical Reduction of N2 to NH3 in Ambient Conditions.

Industrial ammonia production depends heavily on the traditional Haber-Bosch method at the expense of CO2 emissions and large energy consumptions. Artificial fixation of nitrogen to ammonia is therefore regarded as a promising path to yield ammonia in energy-saving conditions. However, a competent electrocatalyst is highly desired, owing to the extremely stable bond of N≡N. In this work, we report Fe2(MoO4)3 nanoparticles as a non-noble-metal electrocatalyst, inspired by nitrogenase enzymes for electrochemically converting nitrogen into ammonia, which achieves a Faradic efficiency of 9.1% and an excellent NH3 yield of 18.16 µg h-1 mg-1 cat in 0.1 M sodium sulfate at -0.6 V vs reversible hydrogen electrode. Also, it has a better ammonia yield rate of 20.09 µg h-1 mg-1 cat in 0.1 M hydrochloric acid. Moreover, this noble-metal-free catalyst exhibits a unique reaction process selectivity and stability compared with the other catalysts working in harsh conditions. The specific reaction processes are analyzed by density functional theoretical calculations to gain insights into the nitrogen reduction reaction (NRR) by this catalyst.

DyF3 : An Efficient Electrocatalyst for N2 Fixation to NH3 under Ambient Conditions.

NH3 synthesis by the Haber-Bosch method is regarded as the dominant method in industry. Such a process is energy-intensive, accompanied by a large amount of CO2 emission. Electrocatalytic N2 reduction is a sustainable avenue for NH3 production at ambient conditions. However, it needs a catalyst to boost the N2 reduction reaction. Here, we demonstrate that DyF3 is an efficient electrocatalyst. In 0.1 m Na2 SO4 , DyF3 attains a large NH3 yield of 10.9 µg h-1 mg-1 cat. at -0.45 V vs. the reversible hydrogen electrode, with the corresponding Faradaic efficiency of 8.8 %. Furthermore, this catalyst exhibits high electrochemical stability.

The synthesis of highly active carbon dot-coated gold nanoparticles via the room-temperature in situ carbonization of organic ligands for 4-nitrophenol reduction.

Due to the serious pollution issue caused by 4-nitrophenol (4-NP), it is of great importance to design effective catalysts for its reduction. Here, a novel and simple strategy was developed for the synthesis of carbon dot-decorated gold nanoparticles (AuNPs/CDs) via the in situ carbonization of organic ligands on AuNPs at room temperature. The enhanced adsorption of 4-NP on CDs via π-π stacking interactions provided a high concentration of 4-NP near AuNPs, leading to a more effective reduction of 4-NP.

Photodegradation Activity of Poly(ethylene oxide-b-ε-caprolactone)-Templated Mesoporous TiO2 Coated with Au and Pt.

Mesoporous TiO2 films are synthesized through evaporation-induced self-assembly using poly(ethylene oxide-b-ε-caprolactone) diblock copolymers as a soft-template. Using small-angle X-ray scattering and scanning electron microscopy, we investigate the effect of the TiO2/PEO-b-PCL ratio on the resulting nanoarchitectonic structure. After sputter-coating Au and Pt layers, these Au/TiO2 and Pt/TiO2 nanocomposite films display drastically enhanced photodegradation of rhodamine 6G under ultraviolet irradiation, due to the metal films inhibiting the rapid recombination of photogenerated charge carriers.

Probing the Intercalation of Noscapine from Sodium Dodecyl Sulfate Micelles to Calf Thymus Deoxyribose Nucleic Acid: A Mechanistic Approach.

Noscapine (NOS) is efficient in inhibiting cellular proliferation and induces apoptosis in nonsmall cell, lung, breast, lymphatic, and prostate cancers. The micelle-assisted drug delivery is a well-known phenomenon; however, the proper mechanism is still unclear. Therefore, in the present study, we have shown a mechanistic approach for the delivery of NOS from sodium dodecyl sulfate (SDS) micelles to calf thymus deoxyribose nucleic acid (ctDNA) base-pairs using various spectroscopic techniques. The absorption and emission spectroscopy results revealed that NOS interacts with the SDS micelle and resides in its hydrophobic core. Further, the intercalation of NOS from SDS micelles to ctDNA was also shown by these techniques. The anisotropy and quenching results further confirmed the relocation of NOS from SDS micelles to ctDNA. The CD analysis suggested that SDS micelles do not perturb the structure of ctDNA, which supported that SDS micelles can be used as a safe delivery vehicle for NOS. This work may be helpful for the invention of advanced micelle-based vehicles for the delivery of an anticancer drug to their specific target site.

Iron phosphide anchored nanoporous carbon as an efficient electrode for supercapacitors and the oxygen reduction reaction.

Inspired by their distinctive properties, transition metal phosphides have gained immense attention as promising electrode materials for energy storage and conversion applications. The introduction of a safe and large-scale method of synthesizing a composite of these materials with carbon is of great significance in the fields of electrochemical and materials sciences. In the current effort, we successfully synthesize an iron phosphide/carbon (FeP/C) with a high specific surface area by the pyrolysis of the gel resulting from the hydrothermal treatment of an iron nitrate-phytic acid mixed solution. In comparison with the blank (P/C), the as-synthesized FeP/C appears to be an efficient electrode material for supercapacitor as well as oxygen reduction reaction (ORR) applications in an alkaline medium in a three-electrode system. In the study of supercapacitors, FeP/C shows areal capacitance of 313 mF cm-2 at 1.2 mA cm-2 while retaining 95% of its initial capacitance value after 10 000 cycles, while in the ORR, the synthesized material exhibits high electrocatalytic activity with an onset potential of ca. 0.86 V vs. RHE through the preferred four-electron pathway and less than 6% H2O2 production calculated in the potential range of 0.0-0.7 V vs. RHE. The stability is found to be better than those of the benchmark Pt/C (20 wt%) catalyst.

Synthesis of Mesoporous TiO2-B Nanobelts with Highly Crystalized Walls toward Efficient H2 Evolution.

Mesoporous TiO2 is attracting increasing interest due to properties suiting a broad range of photocatalytic applications. Here we report the facile synthesis of mesoporous crystalline TiO2-B nanobelts possessing a surface area as high as 80.9 m2 g-1 and uniformly-sized pores of 6-8 nm. Firstly, P25 powders are dissolved in NaOH solution under hydrothermal conditions, forming sodium titanate (Na2Ti3O7) intermediate precursor phase. Then, H2Ti3O7 is successfully obtained by ion exchange through acid washing from Na2Ti3O7 via an alkaline hydrothermal treatment. After calcination at 450 °C, the H2Ti3O7 is converted to a TiO2-B phase. At 600 °C, another anatase phase coexists with TiO2-B, which completely converts into anatase when annealed at 750 °C. Mesoporous TiO2-B nanobelts obtained after annealing at 450 °C are uniform with up to a few micrometers in length, 50-120 nm in width, and 5-15 nm in thickness. The resulting mesoporous TiO2-B nanobelts exhibit efficient H2 evolution capability, which is almost three times that of anatase TiO2 nanobelts.

Nanoarchitectured peroxidase-mimetic nanozymes: mesoporous nanocrystalline α- or γ-iron oxide?

Nanozymes (nanoparticles with enzyme-like properties) have attracted considerable attention in recent years owing to their intrinsic enzyme-like properties and broad application in the fields of ELISA based immunoassay and biosensing. Herein, we systematically investigate the influence of crystal phases (γ-Fe2O3 and α-Fe2O3) of mesoporous iron oxide (IO) on their peroxidase mimetic activity. In addition, we have also demonstrated the applicability of these mesoporous IOs as nanozymes for detecting the glucose biomarker with a limit of detection (LOD) of 0.9 µM. Mesoporous γ-Fe2O3 shows high nanozyme activities (and magnetism) toward the catalytic oxidation of chromogenic substances, such as 3,3',5,5'-tetramethylbenzidine (TMB) and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid)-ABTS, as well as for the colourimetric detection of glucose, compared to that of α-Fe2O3. We believe that this in-depth study of crystal structure based nanozyme activity will guide designing highly effective nanozymes based on iron oxide nanostructures for chemical sensing, biosensing and environmental remediation.