Chemically modified flubendazole carbon electrochemical sensor for aluminum determination in food stuff, Multivitamin syrup and real water samples supported by DFT calculations, IR and morphological tools.

Aluminum is a key component in nearly nourishment stuffs and medications. It is also found in treated drinking water in the form of reactive species, and aluminum salts are commonly utilized as flocculants in water treatment. Meanwhile, it was not thought to be a dangerous metal for people, but research showed a possible link with Alzheimer's disease, breast cancer, autism, and aluminum. Controlling the amount of aluminum in food processing, agriculture, and drinking water is crucial, thus newly synthesized Al(III) ion selective electrode based on innocuous reagent, flubendazole drug, has been developed. The electrode displayed Nernstian slopes of 20.11 0.47 mV decade-1 at 25 ± 1 °C, covering a wide concentration range of Al(III) from 1 × 10-7 to 1 × 10-1 mol L-1. The response mechanism is studied using IR, computational calculations, morphological tools. The developed sensor has been utilized to accurately measure Al(III) ions in genuine water samples, multivitamin syrup, and food stuff.

Enhanced Nanofiltration Process of Thin Film Composite Membrane Using Dodecyl Phenol Ethoxylate and Oleic Acid Ethoxylate for Oilfield Calcite Scale Control.

This research studied the enhancing effect on the nanofiltration composite (TFCNF) membrane of two non-ionic surfactants on a thin-film composite nanofiltration membrane (TFCNF) for calcite scale (CaCO3) inhibition in oilfield application to develop a multifunctional filtration system: nanofiltration, antiscalant, and scale inhibitors. The effectiveness of dodecyl phenol ethoxylate (DPE) and oleic acid ethoxylate (OAE) as novel scale inhibitors were studied using the dynamic method. Scaling tests on the membrane were performed to measure the scaling of the inhibited membrane with and without scale inhibitors for salt rejection, permeability, and flux decline. The results revealed that the TFCNF membrane flux decline was improved in the presence of scale inhibitors from 22% to about 15%. The rejection of the membrane scales increases from 72% for blank membranes, reaching 97.2% and 88% for both DPE and OAE, respectively. These confirmed that scale inhibitor DPE had superior anti-scaling properties against calcite deposits on TFCNF membranes. Inhibited scaled TFCNF membrane was characterized using environmental scanning electron (ESEM), FTIR, and XRD techniques. The results of the prepared TFCNF membrane extensively scaled by the calcite deposits were correlated to its morphology.

Nanofibrous ε-polycaprolactone scaffolds containing Ag-doped magnetite nanoparticles: Physicochemical characterization and biological testing for wound dressing applications in vitro and in vivo.

Skin wounds can lead to numerous complications with dangerous health consequences. In this work, magnetite nanoparticles were doped with different concentrations of antimicrobial silver (Ag) ions and incorporated into the electrospun nanofibrous ε-polycaprolactone (PCL) scaffolds. Nanoparticles and scaffolds with various Ag contents were characterized using a range of physicochemical techniques. Ag entered magnetite as cations and preferentially positioned at tetrahedral sites, introducing lattice distortions and topographic irregularities. Amorphization of the structure due to accommodation of Ag expanded the lattice in the bulk and contracted it on the surface, where broadened distribution of Fe-O coordinations was detected. Promoting spin canting and diminishing the double exchange interaction through altered distribution of ferric and ferrous ions, Ag softened the magnetism of magnetite. By making the nanoparticle structure more defective, Ag modified the interface with the polymer and promoted the protrusion of the nanoparticles from the surface of the polymeric nanofibers, thus increasing their roughness and hydrophilicity, with positive repercussions on cell adhesion and growth. Both the viability of human melanocytes and the antibacterial activity against E. coli and S. aureus increased with the concentration of Ag in the magnetite phase of the scaffolds. Skin wound healing rate in rats also increased in direct proportion with the concentration of Ag in the magnetite phase, and no abnormalities in the dermal and epidermal tissues were visible on day 10 in the treatment group. These results imply an excellent potential of these composite nanofibrous scaffolds for use as wound dressings and in other reconstructive skin therapies.

A highly sensitive, selective and renewable carbon paste electrode based on a unique acyclic diamide ionophore for the potentiometric determination of lead ions in polluted water samples.

Due to the toxicity of lead(ii) to all living organisms as it destroys the central nervous system leading to circulatory system and brain disorders, the development of effective and selective lead(ii) ionophores for its detection is very important. In this work, 1,3-bis[2-(N-morpholino)acetamidophenoxy]propane (BMAPP), belonging to acyclic diamides, was applied as a highly selective lead(ii) ionophore in a carbon paste ion selective electrode for the accurate and precise determination of Pb(ii) ions even in the presence of other interfering ions. Factors affecting the electrode's response behavior were studied and optimized. Scanning electron microscopy (SEM), energy dispersive X-ray (EDX) and FT-IR spectroscopy were used for studying the morphology and response mechanism of the prepared sensor. The lipophilicity of the used ionophore, which contributes to the mechanical stability of the sensor, was studied using the contact angle measurement technique. The selectivity coefficients obtained by the separate solution method (SSM) and fixed interference method (FIM) confirmed the selectivity of the proposed sensor for Pb(ii) ions. The proposed sensor exhibited a Nernstian slope of 29.96 ± 0.34 mV per decade over a wide linear range of 5 × 10-8 to 1 × 10-1 mol L-1 and detection limit of 3 × 10-8 mol L-1 for 2 months with a fast response time (<10 s) and working pH range (2.5-5.5). To further ensure the practical applicability of the sensor, it was successfully applied for the lead(ii) ion determination in different water samples and the obtained data showed an agreement with those obtained by atomic absorption spectroscopy. In addition, it was successfully applied for the potentiometric titration of Pb(ii) against K2CrO4 and Na2SO4.

Novel Triazole Thiole ligand and some of its metal chelates: Synthesis, structure charactertization, thermal behavior in comparison withcomputational caculations andbiological activities.

Structural and molecular properties of HL, 4-amino-5-(2,2-dichloro-1-methylcyclopropyl)-4H-1,2,4-triazole-3-thiol toward the transition metal ions namely Fe(III), Co(II) and Ni(II) had been studied using elemental analyses, magnetic, electronic, FT- IR, 1H-NMR and Thermal analyses (TGA and DTA). The interpretation of thermal decomposition stages had been evaluated. The computations had been done by software of Gaussian 09W package. The geometries of triazole-thiole ligand and its metal chelates were fully optimized using density functional theory B3LYP method. (DFT)/GENECP level by implementing Def2TZVP basis set was used for Fe, Co and Ni-atoms; and basis set 6-311++G (d, p) was used for remainder atoms. There are no symmetry constrains had been applied during geometry optimization. The mixed basis set was selected due to its flexibility. HOMO and LUMO energy values for chelates, chemical hardness and electronegativity had been calculated. NBO calculations had been done at the same level using (NBO 3.1) program involved in the software of Gaussian 09W for measurement qualitatively the intra-molecular delocalization in systems under investigation. The first 15, 85, 65 and 65 low-lying excited states for ligand and Fe, Co and Ni chelates respectively had been calculated within the vertical linear-response. TD-DFT approximation at the same level of theory was used to calculate the electronic absorption spectra of the studied compounds. Their structures are confirmed by successful correlation between experimental and theoretical calculations. The ligand and its metal chelates had been examined against two bacteria such as Gram-positive (Staphylococcus aureus ATTC 12600), GraM-Negative (Escherichia coli ATTC 11775) and two fungus (Aspergillus flavus and Candida albicans) and molecular docking using Auto Dock tools were utilized.

Experimental and theoretical spectroscopic studies in relation to molecular structure investigation of para chloro, para fluoro and para nitro maleanilinic acids.

In the present work novel para chloro, para fluoro and para nitro maleanilic acid derivatives were prepared and investigated using FT-IR, thermal analyses (TA) measurements (TGA/DTG and DTA) in comparison with mass spectral (MS) fragmentation at 70 eV. The crystallographic structures of studied compounds were investigated by X-ray diffraction (XRD). The vibrational frequencies and the corresponding normal modes were evaluated at the optimized geometry. Vibrational modes were analyzed using GAUSSVIEW software. Experimental FT-IR and Raman spectra of the three newly prepared derivatives, namely, (E) - oxo -4- ((4- nitro phenyl) amino)-4- oxobut-2-enoic acid (p-NMA), (E) -4- ((4- chloro phenyl)amino)-4- oxobut -2- enoic acid (p-ClMA), (E) -4- ((4- fluoro phenyl) amino)- 4- oxobut -2- enoic acid (p-FMA) were compared with the theoretically calculated one. FT-IR and the observed vibrational frequencies were assigned; thermal analysis and mass spectrum measurements of the maleanilic acid derivatives were recorded and discussed. The computational calculations were carried out by DFT - B3LYP method with 6-311++G(d,p) basis sets and the corresponding results were tabulated. The alternations of structures of p-FMA, p-ClMA and p-NMA due to the subsequent substitutions were investigated. This correlation between experimental and theoretical calculations provided a good confirmation of the proposed structures of the newly prepared compounds. The derivatives were found to be highly effective against Hepatocellular carcinoma cells > Breast carcinoma cells > colon carcinoma cells. It was recognized, that cancer cells over expression promotes tumorigenic functions; can be suppressed by p-NMA > p-FMA > p-ClMA inhibitors.

Synthesis of novel Schiff's bases of highly potential biological activities and their structure investigation.

Novel bisaldehyde-hydrazide Schiff's bases AS1 (2,2'-(ethane-1,2-diylbis(oxy))dibenzaldehyde terephthalohydrazide) and AS2 (N',N'″-(((ethane-1,2-diylbis(oxy))bis(2,1-phenylene))bis(methanylylidene))di(benzohydrazide)) were prepared as new macrocyclic compounds via condensation reactions. AS1 had been prepared by condensation between (2,2'-(ethane-1,2-diylbis(oxy))dibenzaldehyde) bisaldehyde and terephthalohydrazide in a ratio1:1. AS2 had been obtained by condensation between (2,2'-(ethane-1,2-diylbis(oxy))dibenzaldehyde) bisaldehyde and benzohydrazide in ratio 1:2. The structures of AS1 and AS2 were characterized by elemental analysis (EA), mass (MS), FT-IR and (1)H-NMR spectra, and thermal analyses (TG, DTG). The activation thermodynamic parameters such as ΔE(∗), ΔH(∗), ΔS(∗) and ΔG(∗) were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bonds responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities had been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillus subtilis and Staphylococcus aurous bacteria in order to assess their anti-microbial potential.

Preparation and structure investigation of novel Schiff bases using spectroscopic, thermal analyses and molecular orbital calculations and studying their biological activities.

Two novel Schiff's bases (EB1 and L1) as new macrocyclic compounds were prepared via condensation reactions between bisaldehyde (2,2'-(ethane-1,2-diylbis(oxy))dibenzaldehyde): firstly with hydrazine carbothioamide to give (EB1), secondly with 4,6-diaminopyrimidine-2-thiol to give (L1). EB1 has a general formula C18H20N6O2S2 of mole mass=416.520, and IUPAC name ((N,N'Z,N,N'E)-N,N'-(((ethane1,2diylbis(oxy))bis(2,1phenylene))bis(methanylylidene))bis(1hydrazinylmethanethioamide). L1 has a general formula C20H16N4O2S of mole mass=376.10; and IUPAC name 1,2-bis(2-vinylphenoxy)ethane4,6-diaminopyrimidine-2-thiol). The structures of the compounds obtained were characterized based on elemental analysis, FT-IR and (1)H NMR spectra, mass, and thermogravimetric analysis (TG, DTG). The activation thermodynamic parameters, such as, ΔE(*), ΔH(*), ΔS(*) and ΔG(*) were calculated from the TG curves using Coats-Redfern method. It is important to investigate their structures to know the active groups and weak bond responsible for their biological activities. The obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculation using PM3 procedure, on the neutral and positively charged forms of these novel Schiff bases. Therefore, comparison between MS and TA helps in selection of the proper pathway representing the decomposition of these compounds to give indication about their structures and consequently their biological activities. Their biological activities have been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillissubtilies and Staphylococcus aurous bacteria in order to assess their antimicrobial potential.

Structure investigation of three hydrazones Schiff's bases by spectroscopic, thermal and molecular orbital calculations and their biological activities.

Three Schiff's bases AI (2(1-hydrazonoethyl)phenol), AII (2, 4-dibromo 6-(hydrazonomethyl)phenol) and AIII (2(hydrazonomethyl)phenol) were prepared as new hydrazone compounds via condensation reactions with molar ratio (1:1) of reactants. Firstly by reaction of 2-hydroxy acetophenone solution and hydrazine hydrate; it gives AI. Secondly condensation between 3,5-dibromo-salicylaldehyde and hydrazine hydrate gives AII. Thirdly condensation between salicylaldehyde and hydrazine hydrate gives AIII. The structures of AI-AIII were characterized by elemental analysis (EA), mass (MS), FT-IR and (1)H NMR spectra, and thermal analyses (TG, DTG, and DTA). The activation thermodynamic parameters, such as, ΔE(∗), ΔH(∗), ΔS(∗) and ΔG(∗) were calculated from the TG curves using Coats-Redfern method. It is important to investigate their molecular structures to know the active groups and weak bond responsible for their biological activities. Consequently in the present work, the obtained thermal (TA) and mass (MS) practical results are confirmed by semi-empirical MO-calculations (MOCS) using PM3 procedure. Their biological activities have been tested in vitro against Escherichia coli, Proteus vulgaris, Bacillissubtilies and Staphylococcus aurous bacteria in order to assess their anti-microbial potential.

Synthesis and characterization of SiC and SiC/Si3N4 composite nano powders from waste material.

In the present work, nano silicon carbide has been prepared by pyrolysis of rice-husk ashes as starting materials. Three rice-husk ash samples having different features were used. The first was coarse-grained rice husk ash (fired husk as is), the second was fine rice husk ash (hand-ground), while the third was ball milled one. Effect of ball milling of the starting ashes for 6h on the formation of nano SiC was investigated and compared with those prepared without milling. The particle sizes of the prepared SiC materials were affected by the milling process. The particle sizes of the obtained nano SiC from ball milled staring materials were smaller than those prepared without milling. The pyrolysis conditions, i.e. the temperature and atmosphere were optimized. The optimum firing temperature to obtain well crystalline nano SiC was 1550°C. The effect of pyrolysis atmosphere, i.e. argon, vacuum and nitrogen was also demonstrated. The pyrolysis in argon exhibited lower efficiency on the formation of SiC than vacuum; while the pyrolysis in nitrogen atmosphere led to formation of SiC/Si(3)N(4) nanocomposite.

Enhancement of stabilizing properties of double-base propellants using nano-scale inorganic compounds.

The use of inorganic stabilizers for double-base propellants in literature is scanty; therefore five samples (S(1)-S(5)) of different percentages (2-4%) of nano-clinoptilolite were investigated as new inorganic stabilizers for double-base propellants (DBPs). The grain size of clinoptilolite stabilizer played an important role in the stabilization effect. As the grain size of stabilizer decreases, the surface area of stabilizer increases and the ability to absorb pronounce amount of hazardous nitrogen oxides increases. In this work clinoptilolite in nano-scale (30 nm) has been used to obtain higher stabilizing effect for DBPs. The evaluation process has been performed through the classical thermal stability tests (Bergmann-Junk and calorimetric tests), in comparison with thermal analyses measurements (TGA and DSC) and kinetic parameters calculation such as activation energy (E(a)), enthalpy of activation (ΔH*), Gibbs free energy of activation (ΔG*), entropy of activation (ΔS*) and frequency factor (A), which calculated using Coats-Redfern and Horowitz-Metzger methods. The results for the new stabilizers were compared with that for the classical one (N,N-diethyldiphenyl urea, C(1)). It has been found that the samples containing new stabilizer with percentages (3.0, 3.5 and 4.0%) showed better stability effect for DBPs than the classical one. The efficiency of stabilization of each inorganic stabilizer to DBPs is also rationalized and correlated with its structure.

Spectrophotometric studies of reactions between pseudo-ephedrine with different inorganic and organic reagents and its micro-determination in pure and in pharmaceutical preparations.

Two simple, sensitive, cheep and reliable spectrophotometric methods are suggested for micro-determination of pseudoephedrine in its pure form and in pharmaceutical preparation (Sinofree Tablets). The first one depends on the drug reaction with inorganic sensitive reagent like molybdate anion in aqueous media via formation of ion-pair mechanism. The second one depends on the drug reaction with π-acceptor reagent like DDQ in non-aqueous media via formation of charge transfer complex. These reactions were studied under various conditions and the optimum parameters were selected. Under proper conditions the suggested procedures were successfully applied for micro-determination of pseudoephedrine in pure and in Sinofree Tablets without interference from excepients. The values of SD, RSD, recovery %, LOD, LOQ and Sandell sensitivity refer to the high accuracy and precession of the applied procedures. The results obtained were compared with the data obtained by an official method, referring to confidence and agreement with DDQ procedure results; but it referred to the more accuracy of the molybdate data. Therefore, the suggested procedures are now successfully being applied in routine analysis of this drug in its pharmaceutical formulation (Sinofree) in Saudi Arabian Pharmaceutical Company (SPIMACO) in Boridah El-Qaseem, Saudi Arabia instead of imported kits had been previously used.

Synthesis, characterization and application of enrofloxacin complexes as thermal stabilizers for rigid poly(vinyl chloride).

Synthesis and characterization of both binary Co(II)- (1), Ni(II)- (2) complexes with enrofloxacin drug (HL(1)) and ternary Co(II)- (3), Ni(II)- (4) complexes in presence of DL-alanine (H(2)L(2)) are reported using physico-chemical techniques. The antimicrobial activity of these complexes has been screened against two gram-positive and two gram-negative bacteria. Antifungal activity against two different fungi has been evaluated and compared with reference drug. All the binary and ternary complexes showed remarkable potential antimicrobial activity higher than the recommended standard agents. Ni(II)-complexes exhibited higher potency as compared to the parent drug against bacterial and fungal strain. In addition, it was of interest to investigate the reported complexes as thermal stabilizers and co-stabilizers for rigid PVC in air at 180 °C. Their high stabilizing efficiency is detected by their high induction period values (T(s)) compared with some of the common reference stabilizers used industrially, such as dibasic lead carbonate (DBLC) and calcium-zinc soap. Blending these complexes with some of the reference stabilizers in different ratios had a synergistic effect on both induction period as it gave better thermal stability and lower extent of discoloration. The stabilizing efficiency is attributed at least partially to the ability of the metal complex stabilizer to be incorporated in the polymeric chains, thus disrupting the chain degradation and replace the labile chlorine atoms on PVC chains by a relatively more s moiety of the inorganic stabilizer. Their amenability to use as a biomedical additives for PVC, has afforded them great potential for various medical applications.

Synthesis, structural characterization and antimicrobial activity evaluation of metal complexes of sparfloxacin.

The synthesis and characterization of binary Cu(II)- (1), Co(II)- (2), Ni(II)- (3), Mn(II)- (4), Cr(III)- (5), Fe(III)- (6), La(III)- (7), UO(2)(VI)- (8) complexes with sparfloxacin (HL(1)) and ternary Cu(II)- (9), Co(II)- (10), Ni(II)- (11), Mn(II)- (12), Cr(III)- (13), Fe(III)- (14), La(III)- (15), UO(2)(VI)- (16) complexes with sparfloxacin (HL(1)) and DL-alanine (H(2)L(2)) complexes are reported using elemental analysis, molar conductance, magnetic susceptibility, IR, UV-Vis, thermal analysis and (1)H-NMR spectral studies. The molar conductance measurements of all the complexes in DMF solution correspond to non-electrolytic nature. All complexes were of the high-spin type and found to have six-coordinate octahedral geometry except the Cu(II) complexes which were four coordinate, square planar and U- and La-atoms in the uranyl and lanthanide have a pentagonal bipyramidal coordination sphere. The antimicrobial activity of these complexes has been screened against two gram-positive and two gram-negative bacteria. Antifungal activity against two different fungi has been evaluated and compared with reference drug sparfloxacin. All the binary and ternary complexes showed remarkable potential antimicrobial activity higher than the recommended standard agents. Ni(II)- and Mn(II) complexes exhibited higher potency as compared to the parent drug against gram-negative bacteria.

Synthesis, structure investigation, spectral characteristics and biological activities of some novel azodyes.

Four novel azo compounds were synthesized; o-phenylazo- (C(14)H(13)N(3)O(2)) (I), p-bromo-o-phenylazo- (C(14)H(13)BrN(3)O(2)) (II), p-methoxy-o-phenaylazo- (C(15)H(16)N(3)O(3)) (III) and p-nitro-o-phenylazo-p-acetamidophenol (C(14)H(13)N(4)O(4)) (IV). These compounds were carefully investigated using elemental analyses, UV-vis, FT-IR, (1)H NMR and mass spectra. Also, the effects of p-substituents such as bromo, methoxy and nitro groups on the mass fragmentation pathways of these dyes were studied using Hammet's effects. This research aimed chiefly to threw lights on the structures-stability relationship of four novel newly prepared azo derivatives of p-acetoamidophenol. The data obtained referred to the variation of mass fragmentation pathways with the variation of p-substituent of these dyes which can be used in industry for various dyeing purposes. This variation is also correlated and verified by molecular orbital calculations which were done on ionic forms of these dyes using semi empirical PM3 program. The biological activities of these dyes were also investigated and its structure relationship was correlated.

Spectroscopic study of structure of diphenhydramine drug and its products obtained via reactions with tetracynoethylene and iodine reagents and applications.

The reactions between diphrenhydramine drug (diphen) in the base form and the iodine amphoteric reagent (n-donor and/or σ-acceptor) and tetracyanoethylene as a π-acceptor reagent (TCNE) have been spectrophotometrically studied at different conditions of reactant concentrations, time intervals, temperatures, solvents, and different wavelengths aiming to shed light on the nature of these reactions. Consequently, it is possible to select the proper conditions for spectrophotometric determination of this biologically active drug in its formulations. The reaction mechanism between iodine and diphen involves the formation of diphen-I2 outer-and inner-sphere complexes, whereas diphen-TCNE reaction involves the formation of charge transfer (CT) complex. The analytical parameters of the suggested spectrphometric procedures have been calculated. The values of the Sandell sensitivity, standard deviation (SD), relative standard deviation (RSD) and recovery % refer to the high sensitivity of these procedures applied in analysis of diphen in its formulations. This research also presents a new diphen-I2 promising drug derivative that can be used for the same purpose as its parent. Both diphen-drug and diphen-I2 separated solid product are critically investigated by elemental analyses, FT-IR, ¹HNMR, electron ionization mass spectrometry (EI-MS) and thermal analyses (TA). Practical investigation (TA and MS) data of diphen-drug and its reaction product are confirmed by MO calculations. This research gives a clear idea about the possible metabolites and metabolic pathways of diphen and its derivative in vitro system that may occur in vivo system. The importance of this drug stems from its use as an antihistamine with anticholinergic (drying) and sedative side effects.

Stability studies of double-base propellants with centralite and malonanilide stabilizers using MO calculations in comparison to thermal studies.

Propellants containing nitrate esters need stabilizers to avoid early decomposition or even explosion during storage. Newly prepared malonanilides M1-M5 were tested in stabilizing double-base propellants (DBPs). Their stabilization was compared with the effect of classical stabilizer N,N'-diethyldiphenyl urea (C1) using both practical thermal stability tests (qualitative and quantitative tests) and theoretical molecular orbital calculations. This research shows that the new stabilizers (malonanilides) have good stabilizing effects. Some of malonanilides e.g. (M5) and (M2) have higher stability effects. Different mechanisms were suggested to explain the role of different stabilizers. Molecular orbital calculations using the semi-empirical program AM1 are performed on the new and classical stabilizers. Correlation was made between the volume (ml) of NO(x), weight loss (wt%), other thermal analyses data, calculated thermodynamic parameters like activation energy (E(a), kJ mol(-1)) of the decomposed propellant samples containing different stabilizers and some of their calculated properties such as HOMO, LUMO energies, the charge distribution and the pi-bond order. The stabilization effect decreases with the increase in HOMO energy. The correlation between the net charge and parameters measured for the stabilization effect shows good accordance. Comparison of the results obtained show that the high electron charge on N atom of the stabilizers and on its benzene ring is the most important factor, but not the only factor governing the stabilization effect of the stabilizers.

Biological potential study of metal complexes of sulphonylurea glibenclamide on the house fly, Musca domestica (Diptera-Muscidae): preparation, spectroscopic and thermal characterization.

The ligatation behaviour of sulphonylurea glibenclamide drug is studied in order to give an idea about its potentiality towards some transition metals in vitro systems. Metal complexes of glibenclamide (GCA; H(3)L) drug are prepared and characterized based on elemental analyses, IR, diffused reflectance, magnetic moment, molar conductance and thermal analysis (TG and DTG) techniques. From the elemental analyses data, the complexes are proposed to have the general formulae [M(H(3)L)Cl(n)(H(2)O)(m)].yH(2)O (where M=Cr(III) (n=3, m=1, y=3); Mn(II) (n=2, m=0, y=1); Fe(III) (n=3, m=1, y=0), Co(II) (n=2, m=2, y=0); Ni(II) (n=2, m=2, y=3); Cu(II) (n=2, m=2, y=2) and Zn(II) (n=2, m=0, y=0). The molar conductance data reveal that all the metal chelates are non-electrolytes. IR spectra show that GCA is coordinated to the metal ions in a neutral bidentate manner with OO donor sites of the amide-O and sulphone-O. From the magnetic and solid reflectance spectra, it is found that the geometrical structures of these complexes are octahedral except Mn(II) and Zn(II) complexes which have tetrahedral structure. The thermal behaviour of these chelates is studied using thermogravimetric analysis (TG and DTG) technique. The activation thermodynamic parameters are calculated using Coats-Redfern method. The GCA drug, in comparison to its metal complexes also is screened for its biological activity against house fly, Musca domestica (Diptera-Muscidae). Dose of 5 microg/insect of GCA is topically applied against 3 days old larval instar of M. domestica. Survival of pupal and adult stages has been affected by the complexes of GCA more than larval instars. Morphogenic abnormalities of larvae, pupae and adults are studied. On the other hand pupation and adult emergence program is deteriorated by the effect of different chemicals.

Spectroscopic study of molecular structures of novel Schiff base derived from o-phthaldehyde and 2-aminophenol and its coordination compounds together with their biological activity.

New Schiff base (H(2)L) ligand is prepared via condensation of o-phthaldehyde and 2-aminophenol. The metal complexes of Cr(III), Mn(II), Fe(II), Fe(III), Co(II), Ni(II), Cu(II) and Zn(II) with the ligand are prepared in good yield from the reaction of the ligand with the corresponding metal salts. They are characterized based on elemental analyses, IR, solid reflectance, magnetic moment, electron spin resonance (ESR), molar conductance, (1)H NMR and thermal analysis (TGA). From the elemental analyses data, the complexes are proposed to have the general formulae [M(L)(H(2)O)n].yH(2)O (where M=Mn(II) (n=0, y=1), Fe(II) (n=y=0), Co(II) (n=2, y=0), Ni(II) (n=y=2), Cu(II) (n=0, y=2) and Zn(II) (n=y=0), and [MCl(L)(H(2)O)].yH(2)O (where M=Cr(III) and Fe(III), y=1-2). The molar conductance data reveal that all the metal chelates are non-electrolytes. IR spectra show that H(2)L is coordinated to the metal ions in a bi-negatively tetradentate manner with ONNO donor sites of the azomethine N and deprotonated phenolic-OH. This is supported by the (1)H NMR and ESR data. From the magnetic and solid reflectance spectra, it is found that the geometrical structures of these complexes are octahedral (Cr(III), Fe(III), Co(II) and Ni(II) complexes), tetrahedral (Mn(II), Fe(II) and Zn(II) complexes) and square planar (Cu(II) complex). The thermal behaviour of these chelates is studied and the activation thermodynamic parameters, such as, E*, Delta H*, DeltaS* and Delta G* are calculated from the DrTGA curves using Coats-Redfern method. The parent Schiff base and its eight metal complexes are assayed against two fungal and two bacterial species. With respect to antifungal activity, the parent Schiff base and four metal complexes inhibited the growth of the tested fungi at different rates. Ni(II) complex is the most inhibitory metal complex, followed by Cr(III) complex, parent Schiff base then Co(II) complex. With regard to bacteria, only two of the tested metal complexes (Mn(II) and Fe(II)) weakly inhibit the growth of the two tested bacteria.

Spectroscopic study of the reaction mechanism of buspirone interaction with iodine and tetracyanoethylene reagents and its applications.

The reactions between the drug buspirone (busp) in its base form and iodine amphoteric reagent (n-donor and/or sigma-acceptor) and with tetracyanoethylene as a pi-acceptor reagent (TCNE) have been studied spectrophotometrically at different reactant concentrations, time intervals, temperatures, and with different solvents and wavelengths, with the aim of selecting the conditions that give the most suitable molar extinction coefficients. This study aims chiefly to throw light on the nature of these reactions and to select the most proper conditions for spectrophotometric application of these reagents to determine this biologically active drug used in treating different diseases. The reaction mechanism involves the formation of busp-I(2) outer and inner sphere complexes. The separated busp-I(2) solid product obtained was investigated using elemental analyses, FT-IR, thermal analyses (TA) and electron ionization mass spectrometry (EI-MS) and was found to be biologically active. The reaction mechanism of busp-TCNE involves the formation of a charge transfer (CT) complex. The analytical parameters of the proposed spectrophotometric procedures were calculated. These procedures were applied in the analysis of busp in its formulations as a drug used to treat psychiatric illnesses. The values of the Sandell sensitivity, standard deviation (SD), relative standard deviation (RSD) and recovery percentage show the high sensitivity of these procedures. This study also presents a promising new busp-I(2) drug derivative that can be used more efficiently for the same purposes as its parent. It gives a clear idea about the possible metabolites and metabolic pathways of busp and its derivative that may occur in vivo.