Inkjet-Printed Sensors Based on Nanoferrite-Doped Manganese Oxide Nanoparticles for the Sensitive Differential Pulse Voltammetric Determination of Brimonidine.

The present study described the construction and the electrochemical futures of a novel inject-printed electrochemical sensor based on spinel ferrite-doped manganese oxide nanoparticles (FMnONPs) for the sensitive differential pulse voltammetric quantification of brimonidine (BRIM) in ophthalmic solutions. At the optimized electroanalytical parameters, calibration graphs were linear within the BRIM concentration range of 24-3512 ng mL-1 and recorded a detection limit value of 8.21 ng mL-1. Cyclic voltammograms recorded at different scan rates indicated an adsorption-reaction mechanism for the electrooxidation of BRIM at the electrode surface with the involvement of two electrons and one proton based on the oxidation of the five-membered ring nitrogen atom as recommended by the molecular orbital calculations. The enhanced performance of the introduced inkjet-printed sensors integrated with FMnONPs encourages their application for monitoring BRIM residues in ophthalmic solutions and biological fluids in the presence of BRIM degradation products and other interferents for diverse quality control applications.

Functionalization of Silica Nanoparticles by 5-Chloro-8-quinolinol as a New Nanocomposite for the Efficient Removal and Preconcentration of Al3+ Ions from Water Samples.

In this work, silica nanoparticles were modified by 5-chloro-8-quinolinol as a new nanocomposite for the efficient elimination and preconcentration of Al3+ ions from several water sources. The fabricated composite was characterized utilizing XRD, SEM, FT-IR, TEM, CHN elemental analyzer, and N2 adsorption/desorption analyzer. The XRD demonstrated the existence of a wide peak at 2θ = 30°. Also, all the peaks of silica were severely reduced, which confirms the success of loading the 5-chloro-8-quinolinol on the surface of the silica. The SEM and TEM images demonstrated that the composite resembled cotton, and this confirms that 5-chloro-8-quinolinol was successfully loaded on the silica surface. The specific surface area, the average pore size, and the total pore volume of the synthesized composite are 80.53 m2/g, 3.26 nm, and 0.185 cc/g, respectively. In addition, the greatest uptake capacity of the synthesized composite toward aluminum ions is 95.06 mg/g. The results indicated that the adsorption of aluminum ions onto the silica/5-chloro-8-quinolinol composite follows the Langmuir isotherm and pseudo-second-order model. Moreover, the adsorption of aluminum ions by the silica/5-chloro-8-quinolinol composite is spontaneous, chemical, and thermodynamically favorable. The values of % recovery were more than 97%, whereas the values of % RSD were less than 3.5%. Hence, this confirms the effectiveness of the proposed method in the determination of aluminum ions in real water samples.

Adsorption of Azorubine E122 dye via Na-mordenite with tryptophan composite: batch adsorption, Box-Behnken design optimisation and antibacterial activity.

In the current investigation, we have reported on the preparation of Na-Mordenite (MOR) modified by tryptophan (MOR-NH2) nanocomposite was synthesized and characterized using FT-IR, XRD, SEM, XPS, and BET that represented that the MOR-NH2 has high surface area 288 m2/g and pore volume 0.38 cm3/g. This composite represented high efficiency in removal of food dye Azorubine (E122) was 1043 mg/g. Study all the factors that affected on the adsorption such as pH, dose, salinity, E122 dye concentration as well as study the adsorption isotherm models that represented that was fitted to Langmuir. Moreover, study the effect of time according to it the adsorption process was fitted to Pseudo-second-order, and the effect of temperature that approved that the reaction was endothermic, spontaneous, and chemisorption process. The MOR-NH2 nanocomposite was tested and proven to effectively inhibit the growth of Escherichia coli ATCC® 25922™ and Staphylococcus aureus ATCC® 25923™ at low concentrations. To the best of our knowledge, this work is the first to report the usage of MOR-NH2 adsorbents for the removal of E122 dye in wastewater samples. The mechanism of interaction between MOR-NH2 and E122 dye was determining as it could be through Hydrogen bonding, pore filling, or through π-π interaction. This research offers a promising solution for purifying water sources that are contaminated with a variety of chemicals, microorganisms, and other contaminants.

Green preparation of electrically conductive solution blow spun nanofibers from recycled polyethylene terephthalate via plasma-assisted oxidation-reduction.

Simple and green strategy was described for the development of multifunctional polyester nanofibers (PNFs). Solution blow spinning (SBS) technology was applied to in situ immobilize nanocomposites of polyaniline (PANi) and silver nanoparticles (AgNPs) into plasma-treated polyester nanoscaled fibers prepared. The polyester nanofibers were prepared from recycled polyethylene terephthalate waste, which was exposed plasma-curing and a REDOX reaction in the presence of AgNO3, aniline, and CH3COONH4. Plasma-catalyzed oxidative polymerization of aniline to polyaniline together with a reductive process of Ag+ to silver nanoparticles led to their enduring insoluble dispersion into the surface of polyester nanofibers. By taking the advantage of the PANi oxidation, AgNPs were precipitated from an aqueous medium of AgNPs. The morphological properties were investigated by various analytical techniques. The polyester fiber diameter was determined in the range of 450-650 nm. In addition, transmission electron microscopy (TEM) and scanning electron microscopy (SEM) were utilized to examine AgNPs, demonstrating diameters of 4-20 nm. The plasma-uncured AgNPs/PANi immobilized nanofibrous film displayed weak absorption bands at 399 nm and 403 nm upon increasing the concentration of AgNPs. On the other hand, the plasma-cured AgNPs/PANi immobilized nanofibers displayed strong absorption bands at 526 nm and 568 nm upon increasing the concentration of AgNPs. The AgNP-induced antimicrobial performance and the PANi-induced electrically conductivity were explored. The prepared PNFs showed high UV protection.

Preparation of carbon dots-embedded fluorescent carboxymethyl cellulose hydrogel for anticounterfeiting applications.

Fluorescent inks have been emerged as a desirable encoding technique to enhance anticounterfeiting printing of commercial goods. However, significant drawbacks with fluorescent inks, such as poor durability, low efficiency, and high cost. Herein, we describe the preparation of a self-healing authentication ink based on carboxymethyl cellulose (CMC) hydrogel immobilized with nitrogen-doped carbon dots (NCD) nanoparticles (NPs) for cutting-edge anticounterfeiting applications. Security inks that self-heal are very durable. Under ambient conditions, the prepared NCD@CMC hydrogel could self-heal with a high healing efficiency. It might stick to diverse surfaces such as plastic, glass and paper sheets. The self-healing composite ink demonstrated outstanding photostability under UV light. Straightforward and environmentally friendly method was applied on the agricultural waste of rice straw toward the production of NCD using hydrothermal carbonization in an aqueous medium, and in the presence of NH4OH as an inexpensive passivating agent. The quantum yield (QY) for NCD reached 24.09 %. Various concentrations of NCD NPs were employed to produce self-healable nanocomposite inks with a variety of emission properties. Stamping homogeneous films onto paper surfaces produced a transparent layer. The CIE Lab and emission spectra of prints independently verified the capability of NCD nanocomposite inks to vary their color to blue under UV illumination. To measure the particle diameter of the prepared NCD, their morphological characteristics were examined by transmission electron microscopy (TEM) to indicate diameters of 10-25 nm. Utilizing various analytical techniques, the morphology and chemical composition of the fluorescent prints were examined. We examined the mechanical qualities of the stamped papers as well as the rheological characteristics of the ink hydrogel. Due to their colorless appearance, the excitation band of the printed films was peaked at 364 nm, while their emission was peaked at 465 nm. The current smart ink holds high potential for numerous applications like smart packaging and authentication, and shows great promise as a practical and mass production approach for easily creating anticounterfeiting stamps.

Facile synthesis and characterization of magnesium and manganese mixed oxides for the efficient removal of tartrazine dye from aqueous media.

Nanomaterials are the most effective class of substances for use as adsorbents in wastewater treatment. Hence, the current study involves the facile and low-cost synthesis of MgMn2O4/Mn2O3 and MgMn2O4/Mn2O3/Mg6MnO8 as novel nanostructures from mixed solutions of Mg(ii) and Mn(ii) ions using the Pechini sol-gel method. After that, the remaining powder was calcined at 500, 700, and 900 °C for 3 h; the products were designated as G500, G700, and G900, respectively. The G500 sample consists of MgMn2O4 and Mn2O3, while the G700 and G900 samples consist of MgMn2O4, Mg6MnO8, and Mn2O3. The synthesized nanostructures were characterized using several tools, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and N2 adsorption/desorption analysis. The average crystallite size of the G500, G700, and G900 samples is 210.53, 95.27, and 83.43 nm, respectively. The SEM images showed that the G500 sample consists of square and rectangular bars with an average diameter of 3.18 µm. Also, the G700 and G900 samples consist of hexagonal, polyhedral, and irregular shapes with an average diameter of 1.12 and 0.54 µm, respectively. The synthesized nanostructures were further utilized as adsorbents for the efficient removal of tartrazine dye from aqueous media. The experimental data showed a good fit with the Langmuir isotherm and pseudo-first-order model. The maximum adsorption capacities of the G500, G700, and G900 adsorbents toward tartrazine dye are 328.95, 359.71, and 395.26 mg g-1, respectively.

Preparation of carboxymethyl cellulose/polyvinyl alcohol wound dressing composite immobilized with anthocyanin extract for colorimetric monitoring of wound healing and prevention of wound infection.

Novel aerogel-like wound dressing able to sense the healing progress was developed. Anthocyanins (Ac) have been reported as a significant pH-sensory extract with various biological activities. Herein, anthocyanins were extracted from red-cabbage (Brassica oleracea L. Var. capitata). The anthocyanin probe was integrated as a water-soluble direct dye at various concentrations into carboxymethyl cellulose/polyvinyl alcohol composite in the presence of potassium aluminum sulfate mordant. The generated composites were then freeze-dried to provide the corresponding aerogel-like smart wound dressing to function as an antibacterial and biochromic bulk presenting a comfort dressing biosensor to monitor the progress of a wound healing. Reducing the pH value of a wound mimicking fluid resulted in a hypsochromic shift from 592 to 446 nm. The halochromic activity of anthocyanin showed colorimetric changes from purple to pink. The colorimetric measurements of the prepared anthocyanin-containing aerogel-like diagnostic assay were explored by CIE Lab coordinates and UV-Vis absorption spectra. The effects of the anthocyanin content on the morphology, stiffness, air-permeability, and mechanical behavior of the aerogel-like wound dress were explored by various analytical methods. Both cytotoxicity and antibacterial activity of were investigated.

Synthesis of (tricyanofuran-3-ylmethylene)hydrazinyl thiazole-containing chromophore: A study of its photophysical properties, solvatochromism, and TD-DFT computations.

The chromophore 2-2-(3-cyano-5,5-dimethyl-4-((2-[thiazol-2-yl]hydrazono)methyl)-furan-2(5H)-ylidene)malononitrile (TzHTCF) was prepared by diazo-coupling of diazotized 2-aminothiazole with 3-cyano-2-(dicyanomethylene)-4,5,5-trimethylfuran (TCF). The TzHTCF absorption solvatochromism, in different polarity solvents, demonstrated a ΔEmax = +4.74 in which the positive sign implied the occurrence of a red shift and the TzHTCF lowest excited state was more polar than its ground state. In addition, the TzHTCF fluorescence spectrum produced a λem in the 416-670 nm range and was more dependent on the solvent polarity than the absorption λmax , despite both exhibiting a red shift of 24 and 254 nm, respectively. To discover the Stokes shift ( ∆ ν ¯ ) behaviour of the TzHTCF derivative, Lippert-Mataga and linear solvation-energy relationship (LSER) formulations were utilized in which the LSER approach displayed better results than the Lippert-Mataga method (R2 = 0.9931). Furthermore, the LSER showed that the absorption and fluorescence solvatochromic behaviours were dependent on the solvent's hydrogen-bond donor (α) and acceptor (ß), along with the solvent's polarizability (π*). Moreover, DFT calculations showed that TzHTCF has a planar configuration and its simulated absorption and emission spectra in dimethyl sulphoxide revealed that λmax primarily originated from the HOMO→LUMO and HOMO-1→LUMO transitions, respectively.

Synthesis and characterization of Cu(II)-pyrazole complexes for possible anticancer agents; conformational studies as well as compatible in-silico and in-vitro assays.

New pyrazole derivatives were prepared and used to synthesize new bioactive agents from Cu(II) complexes that have OSN donors. Analytical and spectral (IR, UV-Vis, MS, 1H NMR, ESR & XRD) instruments characterized these complexes as well as their corresponding ligands. The bonding mode has been modified from ligand to ligand and the molar ratio for isolated complexes has also varied (1:1/1:2, M:L). The geometry of isolated complexes was commonly proposed, based on electronic transitions and ESR spectral-parameters. Via computational approaches, these structures were optimized using standard programs (Gaussian 09 & HyperChem 8.1) under the required basis set. Consequently, important physical characteristics have been obtained after finishing the optimization process. Inhibition behavior of all new synthesizes was studied by MOE module as in-silico approach which conducted versus the crystal structure of NUDT5 protein (6gru) of breast cancer cells. The interaction features summarized from docking processes, reveal effective inhibition validity for new Cu(II) complexes versus breast cancer cells. This according to scoring energy values and the stability of docking complexes in true interaction path (bond length ≤3.5 Å) particularly with Cu(II)-L3 and Cu(II)-L4 complexes. This reflects the possibility of successful behavior during practical application through in-vitro assay that intended in this study. Finally, the degree of toxicity of such new compounds to the breast cancer cell line was determined by in-vitro screening. To judge perfectly on their toxicity, in-vitro screening must compared to positive control as Doxorubicin (reference drug). IC50 values were calculated and represent Cu(II) complexes as outstanding cytotoxic agents which revealed superiority on the reference drug itself.

Synthesis of new Cu(II)-benzohydrazide nanometer complexes, spectral, modeling, CT-DNA binding with potential anti-inflammatory and anti-allergic theoretical features.

New nanometer Cu(II)-benzohydrazide complexes were synthesized and characterized. Mono negative tetra-dentate mode is the general feature proposed for all coordinating ligands. Variable structural forms were established, square-planer, tetrahedral and octahedral arrangements around copper centers. XRD and TEM studies displayed a nanometer size for crystalline compounds. TGA analysis of new complexes showed low thermal stability due to the presence of crystal water molecules. Kinetic parameters were calculated using two comparative methods for assertion. ESR study was performed on three chosen complexes to estimate essential spectral parameters and assert on proposed geometries. Gaussian09 software program and applying DFT/B3LYP method was used for optimizing all structures to give the best arrangement for atoms. Essential indexes were extracted from log files as well as other indexes were computed based on frontier energy gaps. Potential theoretical anti-inflammatory, antitumor and anti-allergic studies were executed using Autodock 4.2 tools. Essential energies were calculated over docking complexes corresponding to 5HN1, 5AV1 and 4H1L protein receptors for three pathogens (inflammation, liver cancer and allergy, respectively). H2L5 ligand displays significant activity towards inflammation and allergy diseases. Such potential feature will give a well insight about their biological attitude in future experimentation.

Co-ordination behaviour of a novel tristhiourea tripodal ligand; structural variations in a series of transition metal complexes.

The co-ordination chemistry of a tristhiourea tris(2-pyridylmethyl)amine ligand () with a series of transition metal ions has been investigated. Crystallographic data show that large metal ions, with no geometrical preferences, such as Mn(ii) and Cd(ii), will form seven co-ordinate monocapped octahedral complexes, while smaller metal ions such as Zn(ii) favour five co-ordinate trigonal bipyramidal structures. In a similar manner to the related bisthiourea complexes, the Ni(ii) complex shows a strong preference for octahedral geometries resulting in the ligand binding asymmetrically. Spectroscopic (IR and NMR), spectrometric (MS) as well as electrochemical data for these complexes are reported.

Spectral studies on a series of metal ion complexes derived from pyrimidine nucleus, TEM, biological and γ-irradiation effect.

A series of thiouracil complexes was prepared, all the prepared compounds are investigated by all possible tools. The ligand coordinates towards two central atoms as a neutral hexadentate mode. The octahedral structure was proposed with Ni(II), Pt(IV) and UO2(II) complexes. Square-pyramidal and square planar with VO(II) and Pd(II) complexes, respectively. VO(II) complex was irradiated by using Gamma radiation to through a light on the probability of geometry changes with the effect of radiation. The parameters calculated from ESR spectra before and after γ-irradiation reflect the rigidity of the complex towards the effect. Such may discuss the unaffected biological behavior before and after irradiation. XRD patterns were carried out to emphasis on the nature of the particles and the purity of products. The ligand, Pt(IV) and Pd(II) are found in nanometer range. TEM is a sensitive tool used to justify on the microstructure and surface morphology. All the investigated compounds are in nanorange. TG curves reflect a lower thermal stability of all investigated complexes due to the presence of water of crystallization. Finally, a toxic effect was observed with all investigated complexes towards Gram positive bacterium as well as a resistant behavior was observed with Gram negative bacteria.

Synthesis, spectral, electrochemical and X-ray single crystal studies on Ni(II) and Co(II) complexes derived from 1-benzoyl-3-(4-methylpyridin-2-yl) thiourea.

1-Benzoyl-3-(4-methylpyridin-2-yl) thiourea ligand was coordinated with Ni(II) and Co(II) perchlorate salts to isolate complexes. All the prepared compounds are deliberately investigated by all possible spectral tools. A comparative study for IR spectra reveals the neutral bidentate coordinating nature of the ligand towards the two metal ions. The UV/Vis spectra of the complexes display d-d transition bands proposed an octahedral geometry for the complexes. MS analysis data are concerned especially with the base peak which is corresponding to C28H25N6O2S2 M ion. The fragmentation patterns are relatively matched with each others. Electrochemical studies were carried out using platinum wire and Ag/AgNO3 as counter and reference electrodes, respectively. The data reflect the irreversible nature of the electrode couple and showed two successive one electron transfer process. X-ray single crystal studies are used to verifying the octahedral geometry proposed as well as calculating crystal parameters beside the structural refinements.

Co-ordinative properties of a tripodal trisamide ligand with a capped octahedral preference.

An investigation into the co-ordination chemistry of tris(6-pivaloylamino-2-pyridylmethyl)amine (TPPA) shows a preference for capped octahedral geometry when no additional donors are present. This tripodal ligand yields capped octahedral complexes upon co-ordination to a series of first row transition metals when the counter-ion is a perchlorate, bromide or iodide ion. The exact geometry has been confirmed by shape mapping calculations. The largest variation from the capped octahedral geometry is observed in the case of nickel(ii), indicating a greater octahedral preference of this metal ion.

Synthesis, characterisation and evaluation of a novel copper-64 complex with selective uptake in EMT-6 cells under hypoxic conditions.

The radiometal (64)Cu is now widely used in the development of diagnostic imaging agents for positron emission tomography (PET). The present study has led to the development and evaluation of a novel chelating agent for (64)Cu: the new monothiourea tripodal ligand 1-benzoyl-3-{6-[(bis-pyridin-2-ylmethyl-amino)-methyl]-pyridin-2-yl}-thiourea (MTUBo). X-ray crystallographic analysis has shown this ligand forms a mononuclear complex with copper(II) and co-ordinates via a trigonal bipyramidal N4S array of donor atoms. Promisingly, cell uptake studies revealed that (64)Cu-MTUBo selectively accumulates in EMT-6 cells incubated under hypoxic conditions which may result from its relatively high Cu(II/I) redox potential. Small-animal PET imaging and ex vivo biodistribution studies in EMT-6 tumor bearing BALB/c mice revealed significant tumor uptake after 1 h p.i., yielding tumor-to-muscle (T/M) and tumor-to-blood (T/B) ratios of 8.1 and 1.1, respectively. However, injection of (64)Cu-acetate resulted in similar uptake indicating that the observed uptake was most likely non-specific. Despite showing high in vitro stability, it is likely that in vivo the complex undergoes transchelation to proteins within the blood in a relatively short timeframe. For comparison, the hypoxia imaging agent (64)Cu-ATSM was also evaluated in the same murine tumor model and showed about 60% higher tumor uptake than (64)Cu-MTUBo.

Co-ordination behaviour of a novel bisthiourea tripodal ligand: structural, spectroscopic and electrochemical properties of a series of transition metal complexes.

The synthesis of a thiourea substituted derivative of tris(pyridyl-2-methyl)amine (TPA) is reported. Two of the three pyridine rings are substituted in the 6-position with benzoylthiourea groups. These thiourea groups undergo intramolecular hydrogen bonding to form six-membered rings which leaves one N-H group available to form hydrogen bonds with other molecules. This reports details how the complexation of this new ligand with transition metal ions yields complexes with differing geometries. Seven co-ordinate Mn(II) and Cd(II), six co-ordinate Ni(II) and five co-ordinate Co(II), Cu(II) and Zn(II) complexes have been isolated.

rac-N-{6-[Bromo-(hydr-oxy)meth-yl]-2-pyrid-yl}pivalamide.

The title compound, C(11)H(15)BrN(2)O(2), contains an amide group which is close to coplanar with the adjacent pyridine ring, the dihedral angle between the planes being 9.0 (5)°. The mol-ecular packing reveals a mutual hydrogen-bond inter-action between centrosymmetrically related hydroxyl O atoms. Further hydrogen bonding involving O-H⋯Br and N-H⋯Br inter-actions also appears to consolidate the packing.