: A simple, rapid, accurate, sensitive and eco friendly method has been developed for the quantitative determination of cefixime(CFX) in pure form and pharmaceutical preparations by using a combination of cloud point extraction with UV-Visible absorption spectrophotometric method. Analytical applications of complexation with metal ions by reacting cefixime (CFX) with copper(II) and iron(III) to form chelate complexes under limited experimental conditions. The method based to dissolved CFX in 0.1 M NaOH, 10% (v/v) triton x-114 and mixed with (1000 µ gmL -1 ) copper(II) or (1000 µ gmL -1 ) iron(III). The formation of CFX-Cu(II) complex at pH 13 and wavelength 827 while the complex of CFX-Fe(III) was formatted at pH 11 and wavelength at 439 nm. The complexes of CFX-Cu(II) and CFX-Fe(III) obey Beer’s Law in the range 10-130 and 10-160 µ g/mL respectively. LOD and LOQ values for these complexes were 1.6906 µ g/mL and 5.6355 µ g/mL and LOQ values were 1.58655 µ g/mL and 5.2887 µ g/mL respectively. Method was validated and successfully applied to drug formulations like syrup infusion marketed in Amman and cefixime capsules marketed in Iraq. The results of analysis have been validated statistically by recovery studies and were found satisfactory.
: For the determination of daclatasvir from formulation, a new, simple, specific, accurate and robust isocratic reversed-phase (RP) stability indicating high-performance liquid chromatographic (HPLC) method has been developed and validated. The liquid chromatographic separation isocratically accomplished by means of a portable acetonitrile, buffer (0.1% Octa sulphonic acid) (70:30). The analysis was carried out using at ambient temperature on Xterra C 18 (4.6 x 150 mm, 5.0 µ m) at flow rate of 1 mL/min and the UV detection at 237 nm. The method was validated for accuracy, precision, linearity, range, selectivity and robustness. The linearity of the proposed method was investigated in the range of 20 to 100 µ g/mL ( r 2 = 0.999). The drug was subjected to oxidation, hydrolysis, heat and photolysis to apply stress conditions. The method provided good peak parameters with retention time of 2.398 min. Degradation products resulting from stress studies did not interfere with the detection of daclatasvir and the assay can thus be considered as stability-indicating HPLC method.
: In India, Tigers, Leopards or any wild animals are inhibited in human dominated area to prevent harm to people as well as wild animals. If any wild animals enter in human dominated area, in such cases to save human beings from wild animals like Tigers, generally emergency immobilizations have to be carried with anesthetic drug i.e ., ketamine and xylazine. Usually their mixture is used for immobilization of wild animals. A rare case of Tigress with attempt of immobilization using dart of anesthetic drug was received first time in forensic science laboratory, Nagpur for simultaneous detection of ketamine and xylazine in biological and non biological samples. As per routine toxiclogical analysis of biological (Viscera, Muscle, Skin and blood) and non-biological (Dart with Needle) samples was performed by thin layer chromatography and confirmed by gas chromatography-mass spectroscopy (GCMS). The TLC and GC-MS examination revealed presence of anesthetic drug Ketamine and Xylazine in muscle piece, skin piece and dart with needle.
Tungsten carbide (WC) was synthesized via modified polymer precursor method.The formation of WC was ascertained through Fourier-transform infrared spectra (FT-IR), x-ray diffraction (XRD), thermogravimetry analysis (TGA) and differential thermo analysis (DTA).The WC electrode was synthesized over 316 stainless steel to evaluate electrochemical performance through cyclic voltammetry (CV).The CV curves of WC electrode were found in the potential span of -0.6 to 0.0V in KOH (1.0 M).The WC electrode shows specific capacitance (Cs) of 110 F/g at 0.001 V/s and good cyclic stability over 500 cycles.
: In the present work, CdS nanoparticles were synthesized by four different routes using ammonium sulphide ((NH 4 ) 2 S) as source of (Sulphide) S 2- ions. CdS nanoparticles were grown by simple chemical precipitation reactions in aqueous medium at room temperature. The effect of stabilizers on the stability and size of CdS nanoparticles was studied. The effect of different reaction parameters on the size of nanoparticles, absorbance and respective band gaps and crystalline structure were studied. The microstructure and morphology of the synthesized CdS nanoparticles have been characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. XRD pattern reveals that as-synthesized CdS nanoparticles exhibit both hexagonal and cubic phases. The size of the particles calculated by Debye Scherrer formula according to the XRD spectra has been found to be about 3-30 nm. The optical properties of the sample have been studied by UV-Visible and photoluminescence spectroscopy. The existence of blue shift in UV-Visible spectroscopy reveals the quantum confinement effect of CdS nanoparticles. Finally, the synthesized CdS nanoparticles were exploited for the degradation of acid blue-29 (AB-29), under UV light. The photocatalytic efficiency of the synthesized nanoparticles, using different reaction routes were compared and optimized.
New trinuclear metal complexes of Co(II), Ni(II), Cu(II) and Zn(II) with N-(1Hbenzimidazol-2-yl)-2-mercaptoacetamide (BMA) were synthesized from chloride salts of relative metals in butanol medium.Synthesized metal complexes were characterized by elemental analysis, conductance measurements, IR, UV-Vis, ESR, TGA & DTA and magnetic susceptibility measurements.IR spectral data suggest that the ligand behaves as monobasic tridentate (NOS) with donor sites of azomethine nitrogen (ring), oxygen atom of carbonyl group and thio group.Physicochemical data suggest tetrahedral geometry for Co(II), Ni(II) and Zn(II) complexes.Square planar intended for Cu(II) complex and all these complexes exhibits non-elecrolytic nature.The complexes were evaluated for their antimicrobial activity by in-vitro antimicrobial screening against bacteria Staphylococcus aureus, Bacillus subtilis, Escherichia coli and Klebsiella Pneumonia.The results indicate that antimicrobial activity increased during metallation.A detailed analysis is done theoretically using DFT method with B3LYP/6-311G/LanL2DZ functional for ligand and complexes.Docking studies of ligand and metal complexes carried out using OPLS 2005 force field in Schrodinger suite.
: NiO nanoparticles stabilized with starch was synthesized and characterized using UV-Vis, FT-IR, FESEM and XRD techniques. From FESEM analysis the morphology of the prepared NiO nanoparticles was found to be flower shaped. XRD analysis showed that the NiO nanoparticles corresponds to phase pure cubic crystals and from scherer formula the particle size was calculated to be 9±0.5 nm. Using optical absorption spectra, tha band gap energy was obtained. Photocatalytic activity of the synthesized nanoparticles was investigated by carrying out the degradation studies of norfloxacin under UV light irradiation. In the present work, we have synthesized NiO nanoparticles with biostabilizer starch and used for the photocatalytic degradation of the antibiotic NF. The as prepared NiO nanoparticles are characterized using FESEM, UV-Vis, FT-IR and XRD measurements. Progress of the photo degradation of NF in the presence of NiO nanoparticles was monitored by using time dependant UV-Vis spectra. The reaction followed pseudo first order kinetics. Rate coefficient values at different pH and the optimum pH for degradation of NF was determined.
This work is based on a theoretical study concerning the degradation of basic dyes by advanced oxidation on five basic molecules called as follows: basic red 2 (BR2), basic red 5 (BR5), basic red (BR10), basic violet 5 (BV5) and basic violet 12 (BV12).The purpose of this work is to determine the attack sites most reactive to radical attacks.In other words, the location of the sites which favors the degradation by using the advanced oxidation process.This process is essential in the field of the water depollution.The work was done theoretically by ab initio methods.The calculations were carried out by CAM-B3LYP functional and 6-31++G(d, p) basis set.The exploitation of the results gives the following parameters: local indices of reactivities to radical attacks, global indices of reactivities and transition states.The results obtained from these parameters show the most reactive sites to radical attacks that are in good agreement with the sites determined experimentally.Hence, the majority of the sites were located at the level of the phenazine chromophore constituting the five dyes.
Over the past decade, design of 2-azetidinones scaffold has attracted greater interest of synthesis because of more biological and pharmacological potencies.Specifically, sulfonamide rings and their derivatives represent a medicinally and pharmaceutically important class of heterocyclic motifs that are found as the core structural skeletons in a variety of several naturally occurring alkaloids.We effectively intended 4-(3-chloro-2-oxo-4-aryllazetidin-1-yl)-2 / -(1-(3-ethoxy-4methoxyphenyl)-2-(methylsulfonyl)-ethyl)-2,4′-biisoindoline-1.1′3,3′-tetraones(6(a-f)).4-Amino-2′-(1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethyl)-2,4′-biisoindo line-1, 1′, 3, 3′-tetraone 3 was prepared by condensation of 3-aminophthalic acid 2 with 1,3-ethoxy-4-methoxyphenyl)-2methylsutfonylethylamine 1 by a single step.Condensation of compound 3 with various aromatic aldehydes gives substituted Schiff base of 2′-(1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)ethyl)-2,4′-biisoindoline-1,1′,3,3′-tetraones (5(a-f)) which upon dehydrative annulation in the presence of chloroacetylchloride in the presence of triethylamine in DCM solvent yielded 4-(3-Chloro-2-oxo-4aryllazetidin-1-yl)-2′-(1-(3-ethoxy-4-methoxyphenyl)-2-(methylsulfonyl)-ethyl)-2,4′-biisoindoline-1.1′3,3′-tetraones6(a-f).All the synthesized compounds were recognized by Infra Red-Vibrational spectroscopy, Proton Nuclear Magnetic Resonance, mass spectroscopy and their C, H, N analyses.
A series of of 1,2,3,4-tetrahydro-2-(hydroxyimino)-6-methyl/1,6-dimethyl-4-phenyl pyrimidine-5-carboxylic acid (2a-o) were prepared by refluxing ethyl-1,2,3,4-tetrahydro-6methyl/1,6-dimethyl-2-oxo-4-phenylpyrimidine-5-carboxylate (1a-o) with hydroxylamine hydrochloride in the presence of sodium hydroxide, yielded (2a-o) in excellent yields.The advantages of this method is excellent yields, short reaction time, no side reaction and operational simplicity and ease product isolation The structure of all the synthesized compounds were characterized by FT-IR, 1 H NMR and MS data.The compounds 2a-o has been screened for their antimicrobial activity.All the compounds possesses significant to moderate antibacterial activity and promising antifungal activity.
The current study emphasize about influence of ultrasound irradiation on moderately reactive N,N-dimethylaniline borane (DMAB) towards reduction of organic substrates like carboxylic acids, amides, imine, amino acids, aldehydes, ketones and esters.DMAB conveniently reduces the functional group within 15-25 min of sonication and it does not reduce the ester group even after 300 min of ultrasound irradiation.Besides these reducing properties the DMAB displays chemoselectivity towards different functional group.The amalgamation of borane species from amine borane and ultrasound irradiation provides ecofriendly and expeditious method for the reduction of functional groups.
Zn x Co 1-x Fe 2 O 4 and Mn x Co 1-x Fe 2 O 4 (where x=0.5 atom %) catalysts were synthesized by sol-gel technique and were further characterized by various analytical techniques.PXRD pattern confirms cubic spinel structure for both the samples.UV-Visible spectra show extended absorption in the visible region and the band gap values of Zn 0.5 Co 0.5 Fe 2 O 4 and Mn 0.5 Co 0.5 Fe 2 O 4 catalysts were found to be 1.71 and 1.67 eV.Photocatalytic of experiments show that Mn 0.5 Co 0.5 Fe 2 O 4 is a better photocatalyst compared to the Zn 0.5 Co 0.5 Fe 2 O 4 due to the unique characteristics of Mn 2+ ion which can exist in different oxidation states.
Electrochemical behaviour of cilnidipine at glassy carbon electrode was investigated using cyclic, square wave cathodic adsorptive stripping (SW-CAdS) and differential pulse cathodic adsorptive stripping (DP-CAdS) voltammetry under different experimental conditions. The voltammetric peak current and potential for the reduction of cilnidipine were analysed at different pH, scan rate and concentration. The voltammograms exhibited irreversible reduction of cilnidipine in B R buffer of pH 5.5. Cilnidipine gave one well-defined reduction peak at -0.821 potential versus Ag/AgCl reference electrode in BR buffer of pH 5.5. Reduction process was irreversible and diffusion controlled. Diffusion coefficients (7.45x10 cm/s and 6.45x10 cm/s), surface coverage (4.23x10mol/cm and 98.01x10mol/cm) and heterogeneous rate constant (1.25x10s) were calculated at bare GCE respectively. Based on CV, CPC and pH studies a reduction mechanism was proposed involving 6H/6e. The proposed square wave voltammetric method shows linearity over the concentration range (4.21x10-9.71x10 M) The achieved limits of detection (LOD) and quantification (LOQ) are 5.44x10 g/mL and 1.52x10g/mL respectively.
The molecular structure and reactivity parameters of diphenylguanidine (DPG) were simulated with quantum chemical calculations by using the standard 6-31G**, 6-311++G** and cc-pVDZ basis sets.The bond distance of N1-C2 and N3-C2 are 1.39 Å and 1.42 Å, respectively.The N1-C2 bond posses much more double bond character than the N3-C2 with the longer C-N bond length, though both have partial double-bond character.The molecule exists in the more stable imino form.The C-N bond which connects the aromatic ring has a length of 1.28-1.30Å, close to that of a typical C=N double bond (ca.1.28 Å), and is shorter than the other two C-N bonds of the guanidine.The planarity of the tabiliza group is confirmed from the determined bond angles and torsion angles.The N1-C2-N3 bond angle (109.5°) is always smaller than the other two angles (N1-C2-N4 (123.2 o ) and N3-C2-N4 (127.2 o )).The MEP of the molecule spread in the range +1.224e×10 -2 to -1.224e×10 -2 .The range of total electron density of DPG is +5.545e×10 -2 to -5.545e×10 -2 .The bonding orbital for C2-N3 has 38.07%C2 character in a sp 2.24 hybrid and has 61.93% N3 character in a sp 1.94 hybrid orbital.This clearly reveals the partial double bond character of N1-C2 and C2-N3 bonds.The bond pair donor orbital, π CC → π* CC interaction between the phenyl ring carbon atoms are more tabilizat and the tabilization energy of these interactions lie in the range 16.97-22.78kcal mol -1 .The large total dipole moment of DPG (3.208 D) shows that the polar nature of the molecule.The atoms C2, C13, C22 and C24 are most prone to nucleophilic attack while the electrophilic attack is more on C2, C19 and C12 atoms.The sites C2, C12, C19, C22 and C24 are more susceptible to free radical attack.Fukui dual reactivity descriptor (∆f k ), the dual local softness (∆s k ) and the multiphilicity descriptors (∆ω k ) indicate that the atoms C2, C9, C21 and C22 are more favorable for nucleophilic attack.The atoms N1, N3, C8, C19 and C23 are more favorable for electrophilic attack.
The volumetric behavior of binary mixtures of tetrahydrofuran (THF) +2-methoxyethanol (2-MeOEtOH), + 2-ethoxyethanol (2-EtOEtOH) and 2-butoxyethanol (2-BuOEtOH) were studied at 293.15, 298.15 and 303.15 K to identify the types and strengths of intermolecular interactions taking place in the solvent systems. The densities, ρ, of the pure solvents and the binary mixtures ranging from 0.0003-0.9997 of THF were obtained at the working temperatures. Excess molar volumes, V, of the binary mixtures were calculated from the density data. The calculated excess molar volumes were fitted into the Redlich-Kister polynomial and the fitting coefficients, Ai, obtained. The values of excess molar volumes were negative in all the solvent systems and at all temperatures in the mole fraction region of0.00-0.50 THF. Beyond the mole fraction region of 0.50, the excess molar volumes were slightly positive. The negative excess molar volumes in the region of low THF concentration are attributed to intermolecular hydrogen bonding between unlike molecules of THF and the alkoxyethanols. The magnitudes of the negative excess molar volumes were also found to be dependent upon the chain length of the alkoxy group and the temperature. The results show that the excess molar volumes become more negative when the chain length of the alkoxy group increased and this was attributed to the relative proton-donating ability of the alkoxyethanols investigated.
Two series of Sm/Zr substituted Mg-Mn ferrite materials have been developed having the chemical compositions Mg 0.95 Mn 0.05 Sm 2x Fe 2-2x O 4 and Mg 0.95 Mn 0.05+x Zr x Fe 2-2x O 4 .These materials nanoparticles size ferrites are prepared by using sol-gel method while following ceramic method bulk (larger particle size) ferries are prepared.The value of x varies from 0.0 to 0.5.These are characterized with density, XRD, EDAX, SEM and TEM studies.Based on the obtained results cation distribution is proposed.Samarium is found to occupy B sites while zirconium occupied A and B sites replacing Fe 3+ ions.Density of all the materials found to increase except at higher values of Sm concentration.Lattice parameter of Sm substituted ferrites is found to increase with the rise of Sm content while it decreases with the rise of Zr content.These values obtained due to XRD studies have fair agreement with the theoretically computed lattice parameter values based on the proposed cation distribution.Obtained particle size values due to XRD, SEM and TEM are compared, which are in the nano range.
A series of novel chalcone tethered sulphonamide hybrids 3a-5f were fabricated by condensing appropriate sulphonamide scaffold with methoxy and/or hydroxy substituted chalcones as a multi-target drug for therapeutic treatment.Chalcones were prepared by Claisen-Schmidt condensation of a substituted aldehyde with para aminoacetophenone.The synthesized chalconesulphonamide hybrids were screened by means of their antibacterial activity by NCCLS method.Among all these compounds, 5e and 5c were observed to displaying more potent growth inhibitory activity against bacterial strain and hybrid 5a shows more obvious antifungal activity.FT-IR, NMR and HR-LCMS spectral study assert the structures of synthesized sulphonamide -chalcone hybrids.
: Silicates and related porous materials are solids able to interact with guest molecules, ions and atoms not only at their surfaces but also within the bulk. With the objective of producing materials showing better sorption properties, a laboratory prepared stannic silicate in mixed SnO 2 @SiO 2 form was investigated as potential sorbent for retention of long lived radionuclides 152+154 Eu 3+ from aqueous solution containing 134 Cs + and 60 Co 2+ . Sorption of Eu 3+ has been reported as a function of contact time, initial ion concentration and temperatureat a constant pH equal to 4. The uptake of Eu 3+ was found to be favored at high ion concentration, high temperature and no significant sorption took place after the first 4 h. A pseudo second order kinetic pattern fitted the sorption data well, while equilibrium was positively verified with Freundlich-type equation. Further, in attempt to enhance the separation efficiency of the studied radionuclides from aqueous medium, results showed that the sorption on SnSi was found strongly temperature–dependent. Ions equilibrium was found exothermic in case of 134 Cs + however it endothermic in case of both 60 Co and 134 Cs ions. Based on this contradict uptake, selectivity of ions has been estimated and separation of Eu 3+ from other competing ions was achieved.The thermodynamic parameters ( ∆ G ◦ , ∆ H ◦ and ∆ S ◦ ) showed that the adsorption process is spontaneous and exothermic in case of 134 Cs + but it endothermic in case of the later studied ions.
A novel class of hydantoin derivatives was synthesized and their antioxidant activity was evaluated.The newly synthesized compounds were characterized using 1 H NMR, IR, Mass spectra and elemental analysis.The antioxidant activity of synthesized compounds (3a-d) were examined by 2,2-diphenyl-1-picrylhydrazyl (DPPH), nitric oxide hydroxyl radical scavenging assay.It is revealed from the antioxidant screening results that the compounds 3a and 3d manifested profound antioxidant potential.
A series of 3-n-butylphthlide-edaravone hybrids was synthesized and their structures were elucidated on the basis of analytical and spectral (IR, 1 H NMR, 13 C NMR, MS and elemental analyses) data.These synthesized compounds were evaluated for their in vitro antiplatelet by the turbidimetric method and antioxidant activities by the Fenton method.The results indicated that compound 11a showed similar potency of antiplatelet aggregation as 3-n-butylphthlide and stronger •OH scavenging activity (IC 50 value of 2.87 mM) than edaravone (IC 50 value of 3.57 mM).
