Asian Journal of Chemistry

760-762

Authors: T. Raj Kumar *, S.V. Suresh Kumar and N. Srinivasan

Isoxazoles were synthesized by condensing different aldehydes with 3-aminoacetophenone coupled to N-methyl piperazines. All the compounds were screened for anticancer activity against human breast cancer cell lines- MCF-7 and MDA-MB-468. The antimycobacterial activity of compounds were assessed against M. tuberculosis using microplate alamar blue assay (MABA). The structures of newly synthesized compounds established on the basis of their m.p., TLC, FTIR, mass and 1 H NMR data. The results of antimycobacterial and anticancer studies shows that some of it posses mild to moderate activity against standard. These new synthesized compounds were identified and characterized, demonstrated antitubercular, in vivo efficacy in tumor models like MCF-7 and MDA-MB-468.

767-772

Authors: Duy Trinh Nguyen, Phu Thuong Nhan Nguyen , Thien Hien Tran , Dai Hai Nguyen , Dai Viet N. Vo , Md. Rafiqul Islam , Kwon Taek Lim , Sang Thanh Vo and Long Giang Bach *

A combination of ring-opening polymerization (ROP) and coordination chemistry methodology has been expanded for the synthesis of a multifunctional, biocompatible, magnetic, luminescent nanohybrid complex comprising magnetite (Fe3O4) nanoparticles (MNPs), poly(ε-caprolactone) (PCL) and europium ions (Eu3+). The structural and morphological characteristic of the nanohybrid intricate were studied by appropriate spectrum and physical researches. The superparamagnetic behaviour and unique Eu3+ fluorescence properties with a high emission intensity of MNP-PCL-Eu3+ were investigated via measurements with a superconducting quantum interference equipment magnetism and fluorescence spectroscopy.

780-784

Authors: P. Manimaran and S. Balasubramaniyan*

The metal complexes of Fe(III) and Cu(II) were prepared by using 2,4-dinitrophenyl hydrazine (DNPH) and thiocyanate (SCN) with stirrer refluxed for about 6 h. The prepared Fe(III) and Cu(II) complexes were characterized by elemental analysis, molar conductance, magnetic susceptibility and electronic spectrum, FT-IR spectral studies. The result suggested the octahedral geometry for Fe(III) and Cu(II) complexes. Powder X-ray diffraction indicate the crystalline nature of the metal complexes. The antimicrobial activities of the Fe(III) and Cu(II) complexes were tested with various micro organisms by disc diffusion method. The antimicrobial results indicate that the metal complexes are highly active with compared to the free ligand. The in vitro antioxidant activity of the free ligand and its metal complexes was assayed by radical scavenging activity (DPPH). The result proposed that Fe (III) and Cu(II) complexes exhibited strong antioxidant activity than that of the ligand.

793-798

Authors: S. Karpagavalli *, S. John Kennady Vethanathan and S. Perumal

Hausmannite manganese oxide (Mn3O4) nanoparticles are synthesized by microwave assisted solvothermal method. The calcination temperature of manganese oxide was determined from TG-DTA analysis.The structural characteristics of as prepared Mn3O4 nanoparticles are analyzed by powder X-ray diffraction. The Fourier transform infrared analysis is used to identify molecular structural changes of the manganese oxide sample. The SEM images revealed the surface morphology of the Mn3O4 nanoparticles and determined the size of the particle to be in the range of 30-40 nm. UV-visible spectrum showed that pure Mn3O4 nanoparticle exhibits maximum absorption at 396 nm. The cyclic voltammetry studies are used to evaluate specific capacitance and electrochemical behaviour of Mn3O4 nanoparticles. The magnetic properties of Mn3O4 nanoparticles are examined by vibrating sample magnetometer.

805-812

Authors: Vinay Bharadwaj Tatipamula , Girija Sastry Vedula*, and A.V.S. Sastry

The chemical examination of acetone extract of Dirinaria consimilis resulted in isolation of six depsides of which two novel metabolites namely antarvediside A (1) and antarvediside B (2) and four known metabolites i.e. sekikaic acid (3), atranorin (4), divaricatic acid (5) and 2’-O-methyl divaricatic acid (6). From the pharmacological screening of the isolates (1-6), it was found that 1 and 2 exhibited better inhibition of ABTS and superoxide free radicals than that of the standard and compound 4 showed significant inhibition of protein denaturation with IC50 value of 390 mg/mL with respect to indomethacin with 110 mg/mL. From the SRB assay results, the better IC50 values was determined by compound 2 of 10.5, 11.50 and 12.50 µg/mL on HeLa, MCF-7 and FADU cancer cell lines, respectively. Thus, the outcomes revealed that the D. consimilis is a new source to treat free radicals, inflammation and cancer.

820-824

Authors: Husam S. Khalaf*, , Zainab A.H. Al-Dulaimy , Ahmed M. Abbas and Maida H. Saleem

At the temperature 298.15 K, some physical properties such as: refractive indices (nD), viscosities (η) and densities (ρ) were studied in four liquid-liquid mixtures: carboxylic acids (HCOOH, CH3COOH, CH3CH2COOH and CH3CH2CH2COOH) with tetrahydrofurfuryl alcohol (THFA) with the identified configuration set. These empirical data were utilized to estimate the excess molar volumes (Vm E ), refractive index perversions (∆R), viscosity deviations (ηE ) and excess molar Gibbs free energy (∆G*E). Values of Vm E , ηE , ∆G*E and ∆R were plotted versus mole fraction of tetrahydrofurfuryl alcohol. In all cases, the values of Vm E , ηE , ∆G*E and ∆R that obtained in this study were found to be negative at 298.15 K. The excess parameters were applied in the Redlich-Kister equation by utilizing multi-parameter coefficients that concluded binary coefficients and in respect to the standard deviation. The difference of these characteristics with the formation of binary liquid systems indicates the absence of bipolar bond, variation in the shape and size of component molecules, hydrogen bonding and dipolar interaction among unlike molecules.

829-833

Authors: D.S. Bhagat *, S.G. Pande , M.V. Katariya , R.P. Pawar and P.S. Kendrekar

One-pot efficient protocol to the synthesis of 2-amino-5-oxo-4,5-dihydropyrano(3,2-c)chromene-3- carbonitrile derivatives via condensation of various aryl aldehydes, dicyanomethane and 4-hydroxycoumarin in presence of Emim hydroxide as an excellent homogeneous liquid catalyst. The key advantages of this methodology are mild reaction conditions, novel catalyst, short reaction time, eco-friendly, easy work-up procedure and high yield of isolation of derivatives.

839-844

Authors: Umesh Chandra Sharma *, , Abhishek Kumar Chandra and Sadhana Sachan

Vegetable oils lack acceptable thermo-oxidative stability due to the presence of tertiary β-hydrogen in glycerol backbone of triglyceride molecule. Chemical modification methods may significantly improve the thermo-oxidative stability of vegetable oils derived biolubricants without hindering their environmentally benign characteristics. This study was aimed at evaluation of thermo-oxidative stability of non-edible karanja oil derived biolubricant base oil. The biolubricant karanja oil trimethylolpropane ester (KOTMPE) was synthesized by conventional two step transesterification process. Thermal stability of synthesized product was assessed by thermogravimetric analysis in non-isothermal mode under nitrogen atmosphere, whereas the oxidation stability was analyzed using Rancimat method. Kinetics of thermal degradation of biolubricant was also investigated by thermogravimetric analysis to obtain order of thermal degradation, activation energy and the frequency factor. The results revealed excellent thermo-oxidative stability for synthesized product at high temperatures with ample scope for further improvement by blending with appropriate additives as demanded by specific applications

851-854

Authors: Santhosh Guduru, V.V.S.R.N. Anji Karun Mutha, B. Vijayabhaskar, Muralidharan Kaliyaperumal , Raghu Babu Korupolu , Kishore Babu Bonige and Chidananda Swamy Rumalla *

The stability of aceclofenac under stress conditions was assessed to identify the degradation products. So, it was subjected to stress conditions like acid, base and oxidation, according to ICH guideline Q1A (R2). One degradation product formed when the drug was subjected to acid stress. Three degradation products were formed during the basic stress condition. The drug substance was found to be stable to oxidative stress. The degradants formed during the stress were separated on a C-18 column using gradient preparative HPLC elution. The only product (DP-2) formed during the acid stress and this one is same as of one of the three degradation products (DP-1, DP-2, DP-3) were formed during base stress. 1D and 2D NMR spectra and mass spectral analysis supported the proposed structures for the products. The products DP-2 and DP-3 have been reported earlier but this is the first report of product DP-1 as a degradation product of aceclofenac.

860-872

Authors: F. Mary Anjalin , N. Kanagathara *, M.K. Marchewka and T. Srinivasan

The comprehensive elucidation of the crystal structure, vibrational and Hirshfeld surface analysis of new crystalline product anilinium malonate C6H5NH3 + . C3H3O4 – are presented in this communication. Single crystals of anilinium malonate have been grown by the method of slow evaporation at room temperature. Single crystal XRD study has been carried out to study the structural properties of the grown crystal and it reveals that the crystal crystallizes in the monoclinic system with centrosymmetric space group P2(1)/n. Room temperature powder infrared and Raman spectra of the aniline malonic acid molecular complex (1:1) were carried out. All the characteristic frequencies present in the crystal gives the notable vibrational effect. Hirshfeld surface analysis has been carried out to know the intercontact between the atoms in the structure of the grown crystal

879-885

Authors: Swathi Pon Sakthi Sri V. , A. Vijayakumar and Mary George*

Deep eutectic solvent comprising of choline chloride and D(+)-glucose was synthesized by mixing in the molar ratio 2:1. Iron oxide nanoparticles were successfully synthesized by co-precipitation method. Deep eutectic solvent consisting of D(+)-glucose acts as a promising reducing agent for the synthesis of iron oxide nanoparticles. Direct optical band gap of iron oxide nanoparticles was found to be 2.262 eV. Powder X-ray diffraction technique was used to identify the crystalline phases. Surface morphology analysis by Field emission scanning electron microscopy and high resolution transmission electron microscopy confirmed the rod shape structure of the iron oxide nanoparticles. Selected area electron diffraction pattern revealed the identity of lattice planes with the XRD data. The antibacterial and photocatalytic activities of the iron oxide nanoparticles were also studied. The synthesized iron oxide nanoparticles showed appreciable antibacterial and photocatalytic activities

891-895

Authors: Dinesh Kumar Chelike and K. Juliet Gnana Sundari*

Considering the good corrosion resistance of Zn-Ni alloy, it is selected in the present study to be the protective coating on mild steel and it is considered as a strong candidate for the replacement of environmentally hazardous cadmium. Zn-Ni alloy coating is applied by electrodeposition at optimum temperature, current density and time. The bath solution used is consisting of EDTA as complexing agent. The electrodeposition is also carried out with tartaric acid and benzaldehyde additives to have good corrosion resistance and brightness. The electrodeposits obtained with and without additives are examined for nature and alloy composition. The corrosion behaviour of the electrodeposits is studied by Tafel polarization and electrochemical impedance spectroscopy

901-906

Authors: K. Radhi Devi , G. Selvan , M. Karunakaran * and K. Kasirajan

Pure and metals (Mn & Mg) doped zinc oxide (ZnO, ZnO/Mn and ZnO/Mg) thin films have been successfully grown onto a glass substrates by low cost SILAR method. The structural, morphological, compositional, functional group and optical properties of the prepared films were studied using X-ray diffraction, scanning electron microscope and EDAX, FTIR and UV-visible spectrophotometer, respectively. The structure of the films were found to be hexagonal with polycrystalline in nature with preferential orientation along (002) plane. From Fourier Transform Infrared spectroscopy, the presence of functional groups and its corresponding molecular vibrations were assessed. In UV-visible spectroscopy, the obtained direct optical band gap values 3.46, 3.56 and 3.7 eV for pure, Mn and Mg doped ZnO thin films, respectively. Morphological results showed that the remarkable changes in morphology due to the effect of metal doping. EDAX studies showed that the presence of zinc and oxygen content and also a doping metal ions.

917-924

Authors: K. Dhanalakshmi * , A. Jagannatha Reddy and L. Parashuram

Y2SiO5:Ce3+ (1-7 mol %) nanophosphors were prepared by solution combustion method using oxalyldihydrazide fuel. The phosphors were characterized by X-ray diffraction, scanning electron microscopy, UV-visible and Fourier transform infrared spectroscopy. The XRD patterns confirm the monoclinic structure of the prepared phosphors, with crystallite size of 66-74 nm. The surface morphology and elemental composition were evaluated by SEM and energy dispersive X-ray analysis. The optical band gap was calculated and is between 4.66 eV – 4.9 eV. The presence of Si-O-Si and Y-O bonds was confirmed by the FTIR spectra. Effect of cerium concentration on photoluminescence and thermoluminescence intensity were interpreted. The photoluminescence emission spectrum was recorded under excitation wavelength of 370 nm, the emission spectra showed three significant peaks positioned at 418 nm, 459 nm and 485 nm, which are ascribed to electronic transitions between 5d-4f levels. The nature and activity of trap centers were evaluated from the parameters obtained from Chen′s peak shape method. The intense blue emission by phosphor makes it a competent material for blue emission display devices. Also, its thermoluminescence properties make it a good material for dosimetric applications.

938-942

Authors: S.P. Bhale , A.R. Yadav , S.U. Tekale , R.B. Nawale , R.P. Marathe , P.S. Kendrekar and R.P. Pawar*

Different transition metal complexes were synthesized from novel 3-bromo-2-[1-(4-hydroxy-6-methyl2-oxo-2H-pyran-3-yl)ethylidene]hydrazide ligand (H2L) and characterized by spectral techniques. The synthesized ligand was found to act mono as well as di deprotonated (OH, NH) manner and stoichiometry of the ligand to metal ions was confirmed to be 1:1 in case of complex using metal chloride salts, whereas 1:2 in case of metal(II) complexes using metal acetate(II) salt. Structures of metal complexes were confirmed by IR, 1 H NMR, TGA, XRD, elemental analysis and UV technique which revealed that Mn(II), Co(II), Ni(II), Cu(II) complexes were octahedral geometry and those of Cu(II), Zn(II) showed square planner and tetrahedral geometry around metal ion respectively. Furthermore H2L and its metal complexes were screened for antimicrobial activity which showed that ligand enhanced its biological activity after coordination with metal ions. In particular, Cd(II) and Mn(II) complexes exhibited excellent antifungal activity

951-959

Authors: N.K. Chaudhary*, and B. Guragain

A novel AMXTC2 ligand was prepared by simultaneous stirring and refluxing of an equimolar mixture of amoxicillin and thiophene-2-carbaldehyde in methanol and was further used to synthesize metal complexes by metalation with cobalt and cadmium salts, taking ligand metal ratio 2:1. They were characterized by elemental microanalysis, FT-IR, mass, UV-visible, 1 H NMR, thermal analysis, magnetic moment and molar conductance measurements. The coordination sites in the ligand were verified by their comparative and extensive spectral studies. The detailed exploration of the data suggested octahedral geometry for Co-AMXTC2 and tetrahedral geometry for Cd-AMXTC2 complexes. The thermodynamic and kinetic parameters such as E*, ∆H*, ∆S* and ∆G* of various decomposition steps were calculated from TGA curves using the Coats-Redfern method. The molar conductivity data suggested non-electrolytic nature of the complexes. SEM analysis was done to observe their surface morphology. The geometry optimization of the proposed molecular structure of the complexes was achieved by running MM2 calculation in Gaussian supported Cs-ChemOffice Ultra-11 program software. The biological activities had been evaluated in vitro against E. coli, K. pneumonia, P. vulgaris and S. aureus pathogens in order to assess their antibacterial potency. The biological data revealed better growth inhibitory action of the ligand and metal complexes with bacterial pathogens.

965-970

Authors: Veerabhadrayya S. Negalurmat , Obelannavar Kotresh* and Mahantesha Basanagouda

In the present study, a series of benzofuran-oxadiazole conjugates 7(a-o) was designed, synthesized and characterized through IR, 1 H NMR, 13C NMR and mass spectral data. All the compounds were screened for preliminary antitubercular activity against Mycobacterium phlei and Mycobacterium tuberculosis H37RV. Among all the target compounds, the compound possessing chlorine (7k, MIC 1.56 µg/mL) and bromine (7m, MIC 1.56 µg/mL) on 6th position of benzofuran showed highest activity against Mycobacterium phlei. Whereas, bromine on either 5th position (7l, MIC 3.125 µg/mL) or 6th position (7m MIC 3.125 µg/mL) on benzofuran exhibited highest activity for Mycobacterium tuberculosis (H37 RV).

255-260

Authors: Swathi Thumula

Eco-friendly synthesis of 2-(3H-imidazo[4,5-b]pyridin-2-yl)-N-phenylbenzamide derivatives from diethylphthalate, anilines and pyridine-2,3-diamine was described by one-pot three component method via green approaches. Phosphoric acid has been used as an effective catalyst for this kind of one-pot three component reaction. This reaction takes short time, easy workup and gives excellent yields in glycerol medium

268-274

Authors: Vijaykumar S. Bhamare* and Raviraj M. Kulkarni

The influences of [permanganate], [linezolid], [Ru3+], pH, temperature, ionic strength, solvent polarity, etc. on the rates of uncatalyzed and Ru3+ catalyzed oxidative degradation of linezolid by Mn7+ were investigated at environmentally relevant pH. The increase in [permanganate], [linezolid] and temperature increases the rates of uncatalyzed and catalyzed reactions. It is observed from the calculated pH dependent second order constants that the rate of reaction decreases with increase in pH from 3.0 to 9.0. The values of apparent second order rate constants are 12 times faster in the presence of Ru3+. Four degraded products of linezolid were identified with the help of HR-MS data. Based on kinetic and HR-MS data, a plausible catalytic mechanism was proposed. In this mechanism, Ru3+ acts as an electron shuttle and was oxidized by Mn7+ to the higher oxidation states of ruthenium such as Ru6+ and Ru7+. Activation parameters were determined and discussed.

279-282

Authors: Ashwani Kumar* and Mamta Kamboj

A novel, rapid and facile procedure is described for the determination of vitamin E. It involves the reduction of Fe(III) to Fe(II) with vitamin E that results the formation of pink colored complex of reduced Fe(II) with dimethyl glyoxime in presence of pyridine in pH range between 6.5-7.2. The absorbance of the complex was measured at 512 nm. Beer′s law was obeyed in the range 2.0 to 5.2 µg/ mL of vitamin E with molar absorptivity of 1.23 × 104 L mol-1 cm-1 and the Sandell′s sensitivity was 0.0351 µg/cm2 . The coefficient of determination was r2 = 0.997 with the relative standard deviation 1.1 %. The various factors which affect the resulting complex were optimized to obtain maximum absorption. The proposed method is satisfactorily utilized for pure as well as various dosage forms of vitamin E in pharmaceutical formulations which contains common reductants by pre-treatment of the samples

287-292

Authors: M. Chandrakala*

The Schiff base, 2-salicylidene-4-aminophenyl benzimidazole (I, SAPbzlH) in ethanolic medium reacts with palladium(II) in acidic medium (HCl/HBr) and coordinated SAPbzlH undergoes hydrolysis at -N=CH- bond to yield salicylaldehyde and square planar complexes having composition [Pd(C13H11N3)2X2]·2HX (II) (X = Cl, Br). The obtained complexes have been characterized by elemental analysis, atomic absorption spectra, infrared, electronic and extensive utility of NMR. Possible mechanism for the hydrolysis of coordinated 2-salicylidene-4-aminophenyl benzimidazole (SAPbzlH) has been proposed.

297-302

Authors: Jeevanreddy Miryala, Mahesh Morthad and Satyanarayana Battu*

As a part of our ongoing research in the development of new, selective and environmental friendly methodologies, herein we report a new series of 2-bromo-4-methylthiazole-5-carboxamide derivatives using polyethylene glycol-400 (PEG-400) as a solvent. All the newly synthesized compounds were screened to their in vitro antimicrobial activities and all the compounds exhibited remarkable growth inhibition of wide spectrum of Gram-positive bacteria and Gram-negative bacteria. Molecular docking was done performed computational software GOLD (Genetic algorithm based, flexible ligand, partial flexibility for protein).

309-316

Authors: M. Mesrar , T. Lamcharfi , N.S. Echatoui , F. Abdi and F.Z. Ahjyaje

In this study, the synthesis of ferroelectric (1-x)(Na0.5Bi0.5)TiO3-xBaTiO3 ceramics have been successfully prepared via a hydrothermal process, using bismuth oxide and barium carbonate. The characterization is done using X-ray diffraction, scanning electron microscope, Raman spectroscopy and dielectric measurements. The XRD patterns recorded at room temperature confirmed the formation of a single phase with rhombohedral structure. There is a transformation in crystal structure from rhombohedral to coexistence of rhombohedral and tetragonal to a single tetragonal phase with the increase in BaTiO3 concentration in basic (1-x)(Na0.5Bi0.5)TiO3-x-BaTiO3 composition. From SEM microscopy, the particle sizes are estimated in the range of 5-24 µm. The analysis of both Raman and the spectral deconvolution data of our samples also indicated the distortion of (1-x)(Na0.5Bi0.5)TiO3-xBaTiO3 lattice with the addition of Ba2+ ion. Rietveld refinement method allows us to verify the morphotropic phase boundary at x = 0.05-0.07. The dielectric properties of the solid solution increase with a rise in Ba-TiO3 content and shows optimum value at x = 0.07 owing to the co-existence of two ferroelectric phases. Based on these results, it is proved that morphotropic phase boundary in the studied system is included in the composition x = 0.05 and 0.07.

321-326

Authors: B. Vijaya Kumari*, M. Subbarao and P.V.S. Machi Raju

The mangroves region in East Godavari region of India has its significance and existing as an ecosystem. Anthropogenic activities in the surrounding areas influence the quality of surface as well as ground waters in this region as such there will be a threat to the environment. The present study is focused in characterizing the surface and ground waters to assess the influence of surface waters on ground water quality. Surface and ground water samples were collected from Chollangi mangrove region and characterized for physico-chemical parameters viz., pH, electrical conductivity (EC), total dissolved solids (TDS), total alkalinity (TA), total hardness (TH), calcium and magnesium, sodium, potassium, chloride, sulphate, nitrate and phosphate. The metal ion concentrations were also analyzed by ICP-MS technique. The irrigation parameters like percent sodium (% Na), sodium adsorption ratio (SAR), Kelly's ratio (KR) and magnesium hazard (MH) were determined. The results revealed that the higher value of all the parameters are due to the hectic interactions of surface waters with ground waters, which are a significant cause for contamination of ground waters in the study area. Lower concentrations of metal ions indicate the absence of metal toxicity in waters. However, higher level of magnesium hazard can deplete the soil quality. The presence of bacteria like Pseudomonas spp, E. coli and Bacillus spps can also cause severe health hazards.

333-336

Authors: Chinnadurai Anbuselvan

A series of ((3E,4E)-3,4-bis((pyridin-2-yl)methyleneamino)phenyl)(phenyl)methanone compounds (1-3) were synthesized by a simple one-step condensation reaction of pyridinyl compounds. The synthesized compounds 1-3 were characterized by elemental, FTIR, 1 H and 13C NMR spectral data. From IR and NMR spectra, the characteristic frequencies were assigned and the data used for confirmation of the formation pyridinyl methylene amino. All the compounds were screened for their preliminary antibacterial and antifungal activities. The antimicrobial activity of pyridinyl methylene amino and Schiff bases of pyridinyl substituted compounds were investigated against Staphylococcus aureus, Bacillus cereus and Streptococcus mutans. Gram-negative bacteria (Proteus vulgaris, E. coli, Salmonella typhi) and Candida albicans and Candida tropicalis (fungi). The results indicated that the antimicrobial activity of Schiff bases was stronger than that of pyridinyl compounds and dependent on the substituent group. The pyridinyl substituted compounds 1 and 2 show good antibacterial activity against their bacterial strains within the agreed mm of zone of inhibition. The compounds 1 and 2 substituted pyridinyl also showed good antifungal activities against their fungal strains.

343-347

Authors: S. Archana * and Manjunathan Munisamy

A series of poly(o-phenylenediamine) doped with TiO2 nanoparticles were synthesized by chemical oxidative polymerization method using ferric chloride as an oxidant. The structural, morphological and optical properties were investigated by transmission electron microscope (TEM), FTIR, UV-visible, photoluminescence spectroscopies. It was found that the photoluminescence spectra of polymer nanocomposites emit radiation at 540 nm which corresponds to the emission of green light. The polymer and its nanocomposites exhibit interesting concentration-dependent optical properties.

353-359

Authors: Mouyed Khudhair Hassan and Ahmed Fadhil Khudhair*

For pre-concentration, cloud-point extraction method is used to extract and determine the trace amount of copper element present in urine samples and analyzed by using UV-visible spectrophotometry and flame atomic absorption spectrometry techniques, when copper reacted with salicylaldoxime by using Triton X-114 as non-ionic surfactant to form the complex. The most important factors studied in present work are the order of additions, pH values, the concentration of salicylaldoxime, temperature and appropriate time of extraction process. Other factors studied were the effect of types and concentration of Triton X-114 as non-ionic surfactant. The scatter curve was in the range of 0.50- 16.00 µg/L with r2 = 0.9979 for UV-visible spectrophotometer (λmax = 380 nm). The LOD was 0.103 µg/L. The RSD for six replicates was found to be 4.917 %. This method was applied successfully to determine copper(II) contents in 44 urine samples of occupational workers.

367-372

Authors: U.M. Mandle , L.A. Dhale , Ketan A. Ganure , B.L. Shinde and K.S. Lohar*

Nanocrystalline copper substituted nickel zinc ferrites with composition, Ni0.5CuxZn0.5-xFe2O4 (x = 0.0, 0.1, 0.2, 0.3, 0.4 and 0.5) synthesized by sol-gel auto combustion technique. All the precursors sintered at 400 ºC for 4 h. The stoichiometry and single phase cubic spinel structure confirmed from EDAX and XRD patterns, respectively. Morphology studied by SEM technique. Infrared spectrum of prepared samples investigated at room temperature in the range of 800-300 cm-1. Three major IR absorption bands of tetrahedral frequency in the range of 578-551 cm-1, octahedral frequency in the range of 422-406 cm-1 and ν3 in the range of 352.08 to 325.01 cm-1 observed. The stiffness constant (C11 and C12), elastic moduli, such as Young′s modulus, rigidity modulus, Poisson′s ratio and Debye temperature were determined from IR and structural data. The stiffness constant (C11 and C12) and elastic moduli decreases while Debye temperature increases with copper substitution.

378-384

Authors: P. Jahfar Ali*, S. Elumalai , M. Sathya and G. Muthuraman

Textile industries consume a large quantity of water and generate highly dye contaminated effluents. Textile wastewaters have to be treated or recycled before being discharged. Present work gives a light of extraction, recovery and reuse of methylene blue (MB) a cationic dye; one of the most commonly used substance for dyeing cotton, wood, silk etc., using liquid-liquid extraction method. Even though methylene blue is not only strongly hazardous, it shows some health problems like increased heart rate on acute exposure, shock, vomiting, Heinz body formation, etc. Extraction of methylene blue was carried out using phenol and xylene as carrier and diluent respectively in this work. It was found that extraction increased by increasing the pH of the feed solution and concentration of the carrier. The extracted dye was stripped using acetic acid and found stripping efficiency, increased with increase of acid concentration. More than 99 % dye was extracted with 0.9 mol of phenol and extracted dye was stripped 99 % with 8 N acetic acid. Factors like initial dye concentration, temperature, contact time, the effect of pH, aqueous to organic phase ratio, various stripping agents and different diluents were investigated. Stripped dye and used carrier were reused. FT-IR technique was used to check the reusability of stripped dye.

389-392

Authors: S.S. Kurdur1 , K.A. Thabaj*, R.M. Kulkarni , A.D. Kulkarni , D.P. Rendedula , S.A. Malladi and P.B. Belavi

Oxidative degradation reactions of paliperidone are studied using potassium permanganate in acidic medium spectrophotometrically. Complete reaction was carried out in pseudo first order condition. The reaction orders were calculated with respect to the paliperidone and acid, the obtained values indicate that these reactant have less than first order dependency on the reaction rate. Oxidation products were identified using LC-MS technique and their m/z values were found to be 207, 221 and 443. Kinetics and the mechanism of the reactions were derived from the results identified. The reactions were studied at four different temperatures with different paliperidone and acid concentrations. The activation and thermodynamic parameters were calculated by graphical method.

396-402

Authors: Archana Gautam * and Sulekh Chandra

Complexes of Ni(II), Pd(II), Pt(IV) and Cu(II) with a novel azamacrocyclic ligand viz. 5,7,12,14- tetramethyl-1,2,4,8,10,11-hexaazacyclotetradeca-4,7,11,14-tetraene-3,9-dione (L) were synthesized and characterized by elemental analysis, molar conductance, magnetic susceptibitity, mass spectra, 1 H NMR (L), FT-IR and electronic spectral studies. In molecular modeling, the geometry of ligand (L) was fully optimized with respect to the energy using the 6-31g(d,p) basis set. On the basis of these spectral studies a distorted octahedral geometry was assigned for Ni(II) complex, square planar for Pd(II), octahedral and tetragonal geometry for Pt(IV) and Cu(II) complexes respectively. The ligand and its metal complexes were screened in vitro against some species of bacteria and plant pathogenic fungi. Electrochemical behaviour of nickel and copper complexes were studied by cyclic voltammetry.

410-416

Authors: Hathama Razooki Hasan* and Thikra Hasan Mathkor

Numerous studies have pointed a link between exposure to environmental chemicals and disturbance of hormones. The present study consisted of 22 chemistry undergraduate final year students (11 males and 11 females) of Baghdad University, Iraq. Samples (serum and saliva) were collected in the middle of September, 2017 (before exposure group) and after 3 months of their practical study at chemistry teaching laboratory (after exposure group). All studied hormones (TSH, testosterone and cortisol) were found to increase in both male and female subgroups. The increase was statistically significant for serum TSH and testosterone (p < 0.05) and insignificant for cortisol. Insignificant variations were reported for salivary hormones (testosterone and cortisol). Serum and salivary α-amylase activity was found to be insignificantly decreased and increased respectively, in the exposure groups.

422-426

Authors: Chandrakant V. Zure and Rahul V. Pinjari*

Ethyl-3-methyl-3-phenylglycidate is being used in flavor, fragrance and pharmaceutical industries. Generally acetonitrile, benzene, toluene, methanol and dichloromethane are used as solvent in synthesis of ethyl-3-methyl-3-phenylglycidate. Complete removal of such organic volatile components is not always possible and they may remain at residual level. However, these solvents are harmful and toxic to human as well as in environment above certain concentration. This necessitates the identification of the residual solvents and controlling them within residual solvents acceptance limit set by ICH (Q3C) guidelines. In present work, simple and rapid gas chromatographic method using head space sampler and flame ionization detector have been developed for determination of a residual solvents in ethyl-3-methyl-3-phenylglycidate. This method resulted into a well separation of residual solvents on non-polar capillary columns. The method is validated for precision, recovery, linearity, range and limit of detection as per ICH guideline

433-437

Authors: Siti Umi Kalthum Ab Wahab, Kamaruzzaman Yunus* , Mohd Armi Abu Samah* , Mohd Shukri Mohd Aris and Asnor Azrin Sabuti

This study was focused on the correlation between water quality parameters with the level of radioactive elements and heavy metals at six different sampling points of rivers. For achieving these objectives, collected data was done for Balok river and Tunggak river in dry seasons. Both of the rivers selected were located in Gebeng industrial area, Pahang, Malaysia. The physical parameters such as temperature, specific conductivity, pH, turbidity and dissolved oxygen were measured by using hydrolab. The water samples were then collected for tracing the radioactive elements and heavy metals by using inductively coupled plasma-mass spectrometry (ICP-MS). The readings obtained from both in situ and ex situ analysis was analyzed by using SPSS to know the correlation between water quality parameter, radioactive elements and heavy metals. There were significant relationships found between all water quality parameters and most heavy metals selected (lead and cadmium), except for arsenic. While, for radioactive elements, in the year 2015, there were significant relationships found between most water quality parameters and thorium, exception for uranium. However, for year 2014, there is no significant relationship observed. The findings of the study showed some of the presence of pollutants such as heavy metals and radioactive elements concentrations were reflected some of the water quality parameters at all the sampling locations

445-448

Authors: Abdalfatah Abdalla Fadlelmula* and Abdulaziz Ali Alomari

Capparis spinosa and Dodonaea viscose are commonly known plants in South of Saudi Arabia (Jabal Shuda in Albahah area). They are extremely valued medicinal plants. The variety of active chemicals like flavonoids, tannin and other antioxidants which are responsible of therapeutic properties in these plants, which are vary in their constituents in all plant parts. In this study, the medicinal plants Capparis spinosa and Dodonaea viscose were collected from Jabal Shuda in Albaha Area of Saudi Arabia. Total phenolic content and the effectiveness of the leaves extracts against the free radical scavenging DPPH were carried out. Four different solvents (ethanol, petroleum ether, chloroform, ethyl acetate, and n-butanol) were studied and their results were compared. Total phenolic contents expressed as gallic acid equivalent, whereas scavenging capacity for DPPH radical was measured as IC50 values. The elevated total phenolic content (351.59 ± 0.06 mg/g GAE) and highest value of antioxidant activity (76.58 ± 0.024 % lower value of IC50, 0.0358 ± 0.09 mg/mL) were observed in ethyl acetate extract of D. viscose leaves. The n-butanol extract of C. spinosa leaves exhibited total phenolic content (128.32 ± 0.4 mg GAE/g) which was lower than that shown by n-butanol leaves extract of D. viscose (231.98 ± 0.02 mg GAE/g). Leaves extracts of Capparis spinosa and Dodonaea viscose that grow wildly in Jabal Shuda in Albahah area of Southern Saudi Arabia are rich in phenolic compounds which exhibited high antioxidant activity, but Dodonaea viscose was more valued than Capparis spinosa in these compounds.

453-459

Authors: N. Mahendran, S. Johnson Jeyakumar* , M. Jothibas and A. Muthuvel

The novel HfO2 nanoparticles have been synthesized using sol-gel method. The samples were characterized by X-ray powder diffraction, scanning electron microscopy with elemental analysis, Fourier transform infrared spectrometer, UV-visible spectroscopy. The XRD patterns revealed the transition of cubic to monoclinic phase and calculated particle sizes are 34.92 and 35.66 nm in cubic phase and increase in molar concentration increased the size to 60.31 and 60.33 nm. The optical band gap energy decrease with increasing molar concentrations. We expect that this sol-gel method may be extended to the preparation of nanostructures of other kinds of metal oxides.

463-468

Authors: Chitra Manro* and Ritu Jain

The changes in dielectric parameters of 4-bromoacetanilide in dilute solution of carbon tetrachloride with temperature variation are studied at a fixed frequency of 9.27 GHz. The investigation are being done for five different mole fractions of 4-bromoacetanilide in the microwave region. The values of dielectric constant (ε′) and dielectric loss (ε′′) are determined by using Heston et al. method. Permittivity at a static frequency (εo) and at an optical frequency (ε∞) is calculated with the help of dipole meter and Abbe’s refractometer, respectively. Higasi’s method is used to calculate the values of relaxation times (τ1, τ2 and τ0). From these values, it is found that the relaxation time decreases systematically with the increase in temperature. The fall of τ2 with the increase in temperature has been observed to be more remarkable in comparison to the value of τ1. It indicates that the rate of falls of the relaxation time related to intramolecular rotation with temperature is faster as compared to the internal group rotation.

472-476

Authors: M. Gourouza*, M. Harouna , A. Zanguina , I. Natatou and A. Boos

Niger imports a huge quantity of bentonite, which it uses in mining and oil exploration, but also in village hydraulics. The objective of this study is the search for a bentonite-type clay deposit on the Nigerian territory. The clay fraction of a material collected on a clay deposit of the Paleocene Garadaoua Formation in the Ullemmeden basin (central Niger) was the subject of a series of analyzes: DRX; ICP-AES; ICP-MS; ATD-ATG; IR; Adsorption/desorption of N2 at 77 K; cation exchange capacity, granulometry. DRX results corroborated by those of IR and ATD-ATG indicate that the clay minerals constituting the collected material are: montmorillonite, kaolinite and illite, with a strong predominance of montmorillonite. The mineralogical and chemical composition, the specific surface and the cation exchange capacity obtained indicate that the analyzed material is similar to that of Maghnia bentonite in Algeria.

481-486

Authors: Monika Tyagi and Sulekh Chandra*

Mn(II), Co(II), Ni(II) and Cu(II) complexes with Schiff's base ligand, 3-(benzo[b]thiophen-2- yliminomethyl)-benzene-1,2-diol have been synthesized. All the complexes were characterized by elemental analysis, molar conductance measurements, NMR, mass, IR, EPR and electronic spectral studies. The geometry of complexes has been optimized by using Gaussian 09 W. The complexes were found to be non electrolytes. These complexes have general composition [M(L)2X2] [where L = Schiff′s base ligand, M = Mn(II), Co(II), Ni(II) and Cu(II) and X = Cl− , CH3COO− ]. Spectral data indicates octahedral geometry for Mn(II), Co(II), Ni(II), but Cu(II) complexes were found to have tetragonal geometry. The fungal activity of ligand and complexes has been examined against fungi Aspergillus niger and Candida tropicalis by means of food poison method. The results suggest that the metal complexes show better antifungal activity in the comparison of ligand.

1-8

Authors: Pallavi Jain *, Dinesh Kumar and Sulekh Chandra

Due to their borad profiles of biological activities, transition metal complexes containing semicarbazones and thiosemicarbazones become largely appealing. This mini review focused on the recent developments in last 5 years on the biological applications of Co(II) and Ni(II) complexes of semicarbazones and thiosemicarbazones.

18-24

Authors: S.M. Ho *, M.A. Mahadik , J.S. Jang and V.N. Singh

Thin films have been used for many applications. Hydrogen production from solar water splitting has been considered as a key solution to the energy and environmental issues. The tuned band gap alignments in metal chalcogenides/metal oxides heterostructure enable efficient separation of photogenerated electrons and holes, leading to the effective hydrogen production. We sensitize these structures by hydrothermal methods and evaluate the performance toward hydrogen generation. This work shows a brief overview of photoelectrochemical hydrogen production, progress and ongoing sprints. Here, different metal chalcogenides were deposited on metal oxides (TiO2 and Fe2O3) in order to improve the photoelectrochemical performance by reducing recombination of photogenerated electron–hole pairs and facilitate hole transport at the metal chalcogenides/metal oxides/electrolyte interface. The study includes chalcogenides/metal oxides heterostructure designs and electrochemistry and solar hydrogen generation are brought together, illustrating the promise and challenge of photoelectrochemistry

41-44

Authors: Vijay Kumar Pujari *, Srilalitha Vinnakota , Ramana Kumar Kakarla and Sridhar Marojua

A green one pot synthetic protocol method for 1-(2-chloropyridin-3-yl)-3-substituted urea derivatives from 2-chloropyridin-3-amine and tert-butyl substituted carbamates by using bis(trimethylaluminum)- 1,4-diazabicyclo[2,2,2]octane (DABAL-Me3) under microwave irradiation is developed. The compound structures established by spectral data such as IR, 1 H NMR and mass spectroscopy. All the synthesized compounds were tested in vitro antimicrobial activity.

51-55

Authors: Jai Devi* , Nisha Batra and Jyoti Yadav

Transition metal complexes of cobalt(II), nickel(II), copper(II) and zinc(II) of isatinimine Schiff base ligands (HL1-HL2) derived from isatin 5-chloro-2-hydroxy aniline (HL1), 2-amino-4-nitrophenol (HL2) and heterocyclic nitrogen base 8-hydroxyquinoline have been synthesized. All the metal complexes were characterized by elemental analysis, molar conductance, magnetic susceptibility, SEM and spectroscopic techniques (IR, UV-visible, NMR and ESR). Transition metal complexes existed as octahedral or distorted octahedral geometries around metal centres with the donation of carbonyl oxygen, azomethine nitrogen and deprotonated enolic oxygen, whereas ligand 8-hydroxyquinoline existed as monobasic bidentate ON coordinating through oxygen of hydroxyl group and nitrogen of quinoline ring. The complexes were found to be non-electrolytic in nature.

61-72

Authors: Anil Kumar , Y.F. Nadaf and C.G. Renuka *

The electronic absorption and emission spectra of laser dyes quinoline-390 and rhodamine-800 in distinct organic solvents have been analyzed to understand conventional interactions of solvents on the intensities, peak positions of both absorption and emission spectrum. The relationship between absorption spectrum (λmax) and solvatochromic constants (ε, n, E) indicates that the peak positions are fundamentally influenced by non-specific and specific kind of interactions between the solute and solvent. Solvent effects on the electronic absorption band shift are characteristics of the degree of charge rearrangement of the solute molecules upon electronic excitation. These spectral shifts reflect the effect of the equilibrium solvents association across the energized solute particle, which adjusts inertially as a result of quick charge realignment upon radiative deactivation to the lowest electronic state. Spectral regression study techniques were carried out for the qualitative chemical analyses of these compounds, which provides an opportunity to assess electrical-optical molecular constants within the excited electronic conditions. Further TD-DFT computational techniques for optimized geometry, electronic structure and Mulliken charge distribution in vacuum and ethanol solvent were carried out to acquire additional knowledge of the molecular arrangement and electronic properties of these laser dyes.

79-82

Authors: Balasaheb P. Pagar

The reaction of methylbenzo[h][1,6]naphthyridine (1) with thiourea yield 4-chloro-12-methyl-16,17- dihydro-15-thia-6,11-diaza-cyclopenta[a]phenanthrene-7-thiol (2). The chemistry of compound 2 is explored to obtained iminothioether derivatives (3a-h) in good yields. The structures of newly synthesized compounds were confirmed by spectral data and elemental analysis. The antimicrobial activity of newly synthesized compounds were studied against Staphylococcus aureus, Escherichia coli, Bacillus subtilis, Pseudomonas aeroginosa, Proteus valgaris, Bacillus cereus, Streptococcus sp. and Bacillus megaterium by the agar well diffusion method. Compounds 3d, 3f and 3h showed moderate antimicrobial activity.

89-98

Authors: M.C. Somasekhara Reddy *, K. Sridevi, S.M. Sarvar Jahan and G.V. Subba Reddy

A plant based natural surfactant was extracted from fruit pericarp of Sapindus mukorossi, commonly known as soap nuts. The natural surfactant was used for the treatment of the soils which were contaminated with hydrophobic organic compounds like organic dye, Sudan III and the dye was removed/recovered from the soils. This biosurfactant has great advantages when used in environmental remediation as it is environment friendly in nature. Using a simple water extraction of fruit pericarp powder, the natural surfactant was prepared. The natural surfactant solutions were employed to enhance the aqueous solubility of hydrophobic organic compounds like organic dye, Sudan III and to desorb organic dye Sudan III from contaminated soils in batch experiments. The performance of natural surfactant for the removal of Sudan III was compared with that of commercial surfactants like sodium dodecyl sulphate (SDS) (anionic surfactant), cetyltrimethylammonium bromide (CTAB) (cationic surfactant) and Triton X-100 (TX 100) (non-ionic surfactant). The aqueous solubility enhancement of Sudan III dye in presence of 0.04 M of NaCl was increased in case of non-ionic surfactants like natural surfactant (NS) and TX 100. The solubility of Sudan III dye in presence of 0.04 M of NaCl was decreased in case of ionic surfactants like SDS and CTAB. The desorption behaviour observed for natural surfactant was similar to TX 100 solutions. The natural surfactant solution performance was more or less similar to synthetic surfactants and the removal capacity of surfactant was given in increasing order as TX 100 > NS > SDS > CTAB.

105-108

Authors: Vu Dinh Tien, Vu Van Vu and Tran Khac Vu*

The paper described the preparation of enantiomers of gossypol and apogossypol from racemic gossypol via a two-step procedure. In the first step, D-tryptophan methyl ester was used as an effective agent to resolve racemic gossypol into (–)-gossypol and (+)-gossypol. Next, the deformylation reaction of the corresponding (–)-gossypol and (+)-gossypol was conducted in sodium hydroxide solution, followed by sulfuric acid neutralization in inert atmosphere and the resulting precipitate was filtered and washed with water to give (–)-apogossypol and (+)-apgossypol, respectively in high yields and in high enantiomeric excesses.

114-120

Authors: L.H. Khdium and A.A. Ali Drea*

B3LYP, Lanl2DZ basis sets at density functional theory (DFT) method has been used on a ground state geometry optimized for all proposed structures that have been involved in this study. Structural parameters such as bond lengths, bond angles and dihedral angles have been calculated in the same way to achieve a global reactivity description of Pt(IV) complex. We suggested a minimal energy structure of diaminobis((4-hydroxy-4-butanol)oxy)platinum(IV) chloride complex (DOP) as a new chemotherapy formula of cis-platinum complex. The reactive site of nucleophilic attachment at DOP occurs on carbon atoms due to their positive charge, while other atoms (nitrogen, oxygen, chlorine) are carried negative charges due to the delocalization of electron pair by a resonance effect. Bonds of Pt-Cl with 2.290 Å are more reactive bounds toward the replacement reactions than other chemical bonds in the DOP complex. Investigation revealed that the thermodynamic functions values are increased due to increasing vibrational intensities of cisplatin complex. The fourth transition state (TS4) is the most probable transition state than other suggested transition states for both guanine and adenine bases. The TS4 of platinum complex binding with guanine is the most probable by a factor of -18.134 a.u. of optimization energy value than other suggested states. TS4-guanine is the most probable than other suggested states by factor 7.354 kcal/mol of zero point energy (ZPE). Hence, platinum complex (DOP) is binded with guanine base of DNA through N7

128-134

Authors: S.S. Chine and C.S. Patil *

An efficient method for the synthesis of 1,4-dihydropyridine derivatives from various aryl or heteroaryl aldehydes, β-ketoester and ammonium acetate in presence of laterite catalyst in ethanol under ultrasonication is reported. Catalyst study done with wet chemical analysis, FT-IR, XRD, SEM and EDS techniques. The catalyst can be recovered and reused without noticeable loss of activity even after five cycles.

139-142

Authors: Fatema Tabassum *, Choudhury Mahmood Hasan, Mohammad Mehedi Masud, Sheikh Nazrul Islam and Monira Ahsan

The methanolic extract of the leaves of Ravenia spectabilis was investigated for isolation of secondary metabolites and evaluation of bioactivities. Two alkaloids ravenoline (1) and arborinine (2) were obtained by using vacuum liquid chromatography, gel permeation chromatography and TLC. The compounds were identified by NMR spectroscopy and by comparing the NMR data with those published in the literature. The pure compounds and the petroleum ether, carbon tetrachloride, chloroform and aqueous soluble fractions of the crude methanolic extract of the plant were evaluated for thrombolytic, antioxidant and antimicrobial properties. In the study for thrombolytic property, the pure compounds and different fractions showed thrombolytic activity ranging from 30.43 to 48.85 % as compared to standard streptokinase (74.34 %). All the fractions and the pure compounds showed mild to moderate antibacterial activity. Carbon tetrachloride fraction showed moderate antioxidant activity (97.53 μg/mL) as compared to BHT (27.50 μg/mL), whereas other fractions showed mild antioxidant activity.

148-156

Authors: M. Pragathi * and K. Hussain Reddy

Designing of dinucleating ligands, with an additional donor atom that can bridge two metals in a more or less fixed geometry has rapidly developed in recent years. Part of the interest stems from the fact that the corresponding complexes are often studied as enzyme mimics. Two quinquedentate ligands have been synthesized by condensing salicylaldehyde/o-hydroxy- acetophenone with 2-hydroxy-1,3- propanediamine. The ligands and their metal complexes are synthesized and characterized by physicochemical and spectral analysis. Electrochemical behaviour of the complexes is investigated through cyclic voltammetric studies. E1/2 values are observed at 0.360 and 0.331 V vs. Ag/AgCl for the complexes. The non-equivalent current in cathodic and anodic peaks (ic/ia = 1.224 and 1.065 at 100 mV s-1) for metal complexes indicate quasi-reversible behaviour. Binding interactions of the dinuclear copper(II) complexes with calf thymus DNA are investigated using absorption spectrophotometry. Cleavage activities of these complexes are uncovered on a double stranded pBR plasmid DNA by using gel electrophoresis experiments in different conditions. At micromolar concentration, the ligands exhibit no significant activity, whereas the metal complexes show significantly enhanced nuclease activity due to the presence of metal ions. Copper complexes cleave DNA more effectively in the presence of oxidant. This is consistent with the increased production of hydroxyl radicals by cuprous ions similar to the well known “Fenton reaction”

161-164

Authors: Rajesh Kumar Sharma* and V. Vaijayanthi

Sol-gel technique was used to prepare glasses of the (35-x)B2O3-65Bi2O3-x Fe2O3 (0.1≤ x ≤ 0.4) system (A1-A4: x = 0.1, 0.2, 0.3, 0.4). The local structure and symmetry around trivalent iron were determined by studying X-band powder EPR spectra at room temperature. The EPR spectra of trivalent iron in glass samples are characterized by a more intense line at g = 4.2 and a less intense line at g = 2.0. The EPR line at g = 4.2 is attributed to trivalent iron in rhombic octahedral environment. The line at g = 2.0 is because of two or more trivalent iron coupling through dipole-dipole interactions in distorted octahedral symmetry. The intensity of EPR lines is dependent of Fe2O3 content in the glass samples. At higher concentration of Fe2O3, EPR line at g = 4.2 is less intense whereas the line at g = 2.0 is more intense which is ascribed to the formation of clusters of trivalent iron. The electronic spectra of glass samples show two broad bands corresponding to d-d transition in the range 410-450 nm and in the range 530-570 nm, respectively which are assigned to trivalent iron in distorted octahedral environment

169-175

Authors: D. Rama Rao *, V. Siddaiah and P.V.S. Machiraju

Soil properties are sensitive to various changes in the management and can be employed as indicators. Pollution in soil and water is strictly related to anthropogenic activities such as industrial wastages. Soil is a vital component, medium of unconsolidated nutrients and materials, forms the life layer of plants. The physico-chemical parameters of soil determine their adaptability to cultivation and the level of biological activity that can be supported by the soil. In view of the applications of chemical fertilizers for higher production of crops, the quality of soil decreases. Keeping in view of the rapid industrialization and hectic agricultural activities in East Godavari region of India, there is great need in analyzing the soils for physico-chemical parameters viz. pH, electrical conductivity, total dissolved solids, total alkalinity, CO3 2–, HCO3 –, OH–, total hardness, Ca2+, Mg2+, Na2+, K+, chloride, sulphate and phosphate to assess the chemical contamination of soils. The correlation matrices for physicochemical parameters are generated to verify the internal relationship between the parameters. Further it is also proposed to estimation of the irrigation parameters viz., percent sodium (Na %), sodium adsorption ratio (SAR), Kelly's ratio (KR) and magnesium hazard (MH) to verify the suitability of soils for irrigation purposes. The results revealed that the soils near sago, paper and sugar industrial areas are slightly alkaline in nature. Higher phosphate concentration indicates the discharge of agriculture runoff in to soils. These irrigation parametric values indicate that these soils suitable for irrigation purposes however higher magnesium hazard (MH) values of soil indicate the depletion of the soil quality which in turn reduce the yield of the crops in study areas.

181-185

Authors: Ekhlas Sheakh Aldeen, Tilal Elsaman *, Malik Suliman Mohamed, Mohamed E. Adam and Magdi Awadalla Mohamed

In the present investigation, 6 compounds (E1-E6) were synthesized by reaction of ethyl esters of p-substituted benzoic acid with hydroxylamine. The chemical structures of the synthesized hydroxamic acids were verified on the basis of spectral analysis (IR, 1H NMR, 13C NMR and mass spectra). The benzohydroxamic acids were examined for potential local anesthetic activity using foot withdrawal reflex of the frog and benzocaine was used as standard drug. Compounds were tested at two different solvents; 5 % DMSO and 0.65 % NaOH, each solution was tested at three different concentration levels (40, 100 and 200 μg/mL). Local anesthetic activity of the compounds differed according to the concentration level and selected solvent. Compounds E4 and E5 were found to be the most active and were comparable to the standard drug in tested solvents at all investigated concentrations. All compounds displayed an enhanced activity in the the aqueous basic solutions

191-198

Authors: L. Devaraj Stephen1, S.G. Gunasekaran1, G. Nalini2 and M. Soundarrajan1,*

Medium imparts changes in redox reactions of metal complexes. That is, solvent plays an important role in trapping the exchanging electron on one site similar to that of intramolecular structural changes. Especially in ionic reactions, ion can be thought of creating a polarization field in the surrounding solvent. The rationality behind the proposal of the kinetics was detailed by fit the data in correlation equation involving linear and multiple Grunwald-Winstein plot, Swain’s dual linear relationship and Kamlet-Taft’s equations. The kinetic inferences of outer-sphere electron transfer reactions of cobalt(III) aryl amine complexes (CoIII(pn)2Cl(L)2+ where L = RC6H5NH2, R = m-OCH3, p-F and H) with MeOH/ dioxane solvent content were explored at different temperatures.

213-219

Authors: Nitin S. Pagar * and Raj M. Deshpande

The hydroformylation of terpenes has been studied with homogeneous Rh, Co and Pt complexes. The rhodium complex, Rh(CO)2(acac) modified with triphenyl phosphite ligand has been found to be the best catalyst system for hydroformylation of camphene and other terpenes. The role of ligands, solvents, Rh:P ratio and reaction conditions on the activity and selectivity towards camphene hydroformylation have been investigated.

229-234

Authors: Mohamad Mirzan, Karna Wijaya *, Iip Izul Falah and Wega Trisunaryanti

Bentonite as a carrier was modified by means of pillarization using ZrOCl2·8H2O pillaring solution. Calcination was performed to obtain ZrO2 bounded bentonite. To create a bifunctional catalyst, ZrO2- bentonite was impregnated using Ni(NO3)2·6H2O precursor as nickel metal source. Subsequently, calcination and reduction steps were performed to obtain Ni/ZrO2-bentonite catalyst. The physicalchemical properties of catalyst was characterized by XRD, XRF and the surface area was analyzed with BET, surface acidity with gravimetric method using NH3 vapour, FT-IR and TEM. The characterized results by XRD showed specific peaks of montmorillonite mineral still visible after the pillarization and impregnation process with nickel metal. The XRD analysis also showed an increase in basal spacing d001 of the catalyst sample after the pillarization process characterized by the shifting of specific peaks d001 to the left (2θ < 5º). The XRF analysis showed that the nickel content in bentonite sample was increased after impregnation with the Ni(NO3)2·6H2O precursor. Qualitatively, acidity of the catalysts was determined by FTIR showing characteristics for Brønsted and Lewis acids at wavenumbers 1635-1381 cm-1. Surface area analysis results showed an increase in specific surface area after pillarization and impregnation with nickel metal.

247-250

Authors: Firas H. Abdulrazzak, Ahmed M. Abbas and Falah H. Hussein*

Multi-walled carbon nanotubes (MWNTs) were synthesized from Iraqis natural gas using flame under carbon monoxide atmosphere. The study focuses on abilities to synthesis and characterization of carbon nanotubes (CNTs) using simple, easy, low cost by natural material. The reactor has been designed for synthesis of carbon nanotubes CNTs from natural gas which acted as a source of carbon in addition to supplying thermal energy instead of electrical energy. Crystallographic and morphological of CNTs have been characterized using powder X-ray diffraction, Raman spectroscopy, transmission electron microscope and thermal gravimetric analysis. The analysis refers to synthesized MWNTs with purity 57.80 % and outer diameter 6.6-17.9 nm, inner diameter 3.2-6.3 nm which equal to 3-9 of graphene layers while the length of tubes is 0.8 to 2 μm.

1889-1894

Authors: Vishwa Deepak Tripathi

Present work demonstrates a facile synthesis of a series of 20 dihydropyrazole derivatives from well designed curcumin analogues by reaction of chalcone derivatives with phenylhydrazine. All the synthesized compounds were characterized by spectroscopic (1 H and 13C NMR, IR spectra), spectrometric (Mass spectra) data and elemental analysis. Synthesized dihydropyrazoles have diversity points on attached phenyl ring. Effect of substituent on reactivity was explained on the basis of electronic effect generated due to groups on phenyl ring. Presence of dd (double doublet) in 1 H NMR spectrum of dihydropyrazoles was also explained due to presence of optically active carbon of pyrazole ring

1899-1904

Authors: K. Subashini1,2, S. Prakash1 and V. Sujatha1

There are many methods to synthesize metal and metal oxide nanoparticles. In this paper, copper oxide nanoparticles have been synthesized by solution combustion method using Brassia actinophylla i.e. Schefflera actinophylla flower extract belongs to Araliaceae family. The importance of solution combustion is one of the easy and simplest methods for the synthesis of metal oxide nanoparticle. The CuO nanoparticles were synthesized at various temperatures and the characterization has been carried out by UV, FTIR, PXRD, SEM, TEM and EDAX analysis. At lower temperature, the peak was not observed but at 400 ºC, the UV peak was observed at 340 nm. The FTIR peaks observed at 1000-500 cm-1 confirms again the presence of CuO nanoparticles. The monoclinic phase and crystalline structure of nanoparticles were revealed by PXRD pattern, by Scherrer′s method the average crystalline sizes were found to be in the range of 15 to 24 nm. The size and the shape of nanoparticles were confirmed by SEM and TEM reports. The SEM images of nanoparticles show spherical in shape and free from agglomeration. TEM analysis reports the nanoparticle sizes ranging from 2 to 20 nm. The percentage of copper (52 %) and oxygen (26 %) elements were recorded in the EDAX analysis. The study of size and stability of nanoparticles were done by zeta potential values. The antibacterial activity of CuO nanoparticles were carried out against Staphylococcus aureus and Escherichia coli bacteria's by agar well diffusion method. The MTT assay was performed in order to check the anticancer activity of CuO nanoparticles against HT-29 colon cancer cells.

1913-1918

Authors: Ch. Sanjeeva Reddy, A. Nagaraj , V. Yakub and B. Kalyani

A series of novel 3-4-[2-hydroxy-5-(4-hydroxy-3-2-[2-(aryl)-4-oxo-1,3-thiazolan-3-yl]-6-phenyl-4- pyrimidinylbenzyl)phenyl]-6-phenyl-2-pyrimidinyl-2-(aryl)-1,3-thiazolan-4-ones 5(a-j) have been synthesized and assayed for their antibacterial activity against B. subtilis, B. sphaericus, S. aureus, P. aeruginosa, K. Aerogenes and C. violaceum. The inhibition zones and minimal inhibitory concentrations were measured and compared with the streptomycin. The antibacterial screening data reveal that the compounds containing 4-nitrophenyl (5c), 3-nitrophenyl (5d), 4-dimethylaminophenyl (5g) and 1,3-benzodioxole (5j) moiety at 2-position of the thiazolidin-4-one ring exhibited potent inhibitory activity towards all the tested microorganism, which is higher than streptomycin. The other compounds also showed moderate to good activity

1926-1930

Authors: Veenu Chugh , Sangeeta Sharma and Rimpi Mehani Ne'e Chopra

This paper describes the synthesis, spectral studies and antimicrobial properties of the complexes with the formula [M(C30H24N4O2)Cl2], where M = Fe(II), Co(II), Ni(II), Zn(II) and Cu(II). These complexes were prepared by yield effective template condensation of hexamethylenediamine and 2,2-dihydroxyindane-1,3-dione(ninhydrin). The synthesized complexes were characterized by elemental analysis, infrared spectra, thermogravimetric analysis, Mass spectrum, 13C NMR, molar conductance, electronic spectra, magnetic measurements. TGA and X-ray diffraction studies were used to ascertain the crystal structure and thermal stability of the complexes. The antimicrobial properties of complexes against two Gram-positive bacteria and two Gram-negative bacteria were evaluated by Agar well diffusion technique. Streptomycin and chloramphenicol were taken as standard antibiotics. The results shows that some of the complexes have potential to act as antibacterial agents

1943-1948

Authors: Priyabrata Mohanty1 , Tapan Kumar Bastia1,*, Dibakar Behera1 and Shivkumari Panda

This work represents the preparation and characterization of some unique properties of vinyl ester (VE) and unsaturated polyester (UPE) blend based nanocomposites by introducing biopolymer chitosan grafted multi-walled carbon nanotubes (MWCNTs). Initially, surface grafting of MWCNTs with chitosan was performed by utilizing glutaraldehyde as a cross linking reagent through covalent deposition method and are successfully characterized by Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy(SEM). Then 50:50 wt % of vinyl ester and unsaturated polyester blend was prepared by simple sonication method. Three different specimens of VE/UPE/CS-g-MWCNTs nanocomposites were fabricated with addition of 1, 3 and 5 wt % of functionalized bionanofiller. Chitosan grafting of MWCNTs offered enhanced properties to the nanocomposites suggesting homogeneous distribution of the nanofiller in the matrix with minimum corrosion and swelling properties. 3 wt % of functionalized bionanofiller loading showed superior essential characteristics and after that the properties reduced may be due to the nucleating tendency of the nanofiller particles.

1959-1965

Authors: M. Meghna , B. Athira, T.S. Saranya and Asha Asokan Manakadan

Alzheimer’s disease is a progressive neurodegenerative disorder, is the common cause of dementia and affect life quality. Present research analysis is based on the amyloid precursor protein as it is one of the major biomarkers of Alzheimer’s disease, the insoluble part of which gets deposited due to the inappropriate cleavage by secretase enzyme. The instrumental part of this study was performed by using Computer Aided Drug Design (CADD). About 23 phytoconstituents were taken, from these constituents rosamarinic acid produced the highest docking score. Preliminary characterizations of all the ligands were conducted using Biovia Discovery studio along with protein characterization, Lipinski rule analysis and ADMET. The in silico analysis convincingly predicted the action of rosamarinic acid, against the formation of amyloid plaque by binding with the amyloid precursor protein .Details of single nucleotide polymorphism on gene APPI were analyzed by dbSNP database and displays the need for further in vitro study.

1971-1978

Authors: S.R. Kande1 , U.G. Ghoshir1 , J.K. Khedkar2 , G.G. Muley3 and A.B. Gambhire4,*

Boron (B), carbon (C) and sulphur (S) doped ZnO-SnO2 were successfully prepared by facile precipitation method. As prepared nanocomposite photocatalyst was characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, high resolution transmission electron spectroscopy, Fourier transform infrared spectroscopy, photoluminescence spectra, UV-diffuse reflectance spectra and BET surface area measurement. The photocatalytic activity of prepared nanocomposite photocatalysts was studied by degradation of methyl orange dye under natural sunlight irradiation. S-doped ZnO-SnO2 was found to be more efficient than that of B,C-doped ZnO-SnO2 and bare ZnO-SnO2 nanocomposites. The photocatalytic activity of prepared photocatalysts follows trend as: S-doped ZnO-SnO2 > C-doped ZnO-SnO2 > B-doped ZnO-SnO2 > pure ZnO-SnO2. The enhanced activity of prepared photocatalysts could be attributed to the high specific surface area and small particle size.

1985-1988

Authors: Indah Hairunisa1 , Muhammad Da'i2 , Erindyah Retno Wikantyasning2,*, Andhika Rizky Gilang Mahaputra2 , Normaidah Normaidah3 and Mohd Fadzelly Abu Bakar

Determination of major bioactive compounds in polyphyto-formulation is important for production of standardized herbal products. A fast, simple and inexpensive method for detection and quantification of andrographolide concentration in nanoemulsion preparations containing a combination of Andrographis paniculata (Burm f.) Ness. and Phyllanthus niruri L. has been developed. Detection and quantification were carried out using UV-vis spectrophotometry analysis with picric acid reagent and NaOH (8:2) in methanol solvents, read at maximum wavelength 479 nm with 22 min of incubation time. Validation was done by determine the parameters such as linearity, intra and interday precision, accuracy, limit of detection (LOD) and limit of quantification (LOQ). The results obtained showed linearity with r = 0.9945 (y = 0.0109x − 0.2066) in the range of 30-80 µg/mL. The accuracy (recovery) varied in the range of 97.15 to 104.42 %. Percentage of relative standard deviation (% RSD) for precision and intermediate precision value were 3.23 and 3.02 % with LOD value 211 µg/mL and the LOQ 705 µg/mL. As a conclusion, this method is suitable to detect andrographolide content in herbal nano-preparation.

1993-1999

Authors: Reena Saritha Serrao, S.Z. Mohamed Shamshuddin and Joyce D'souza

A series of solid acid catalysts such as ZrO2, Mo(VI)/ZrO2 and W(VI)/ZrO2 have been coated on honeycomb monoliths as well as synthesized in the powder forms and used as catalytic materials for synthesis of ethyl levulinate from levulinic acid and ethanol. These solid acids were characterized by BET, NH3-TPD/n-butyl amine back titration, FTIR, PXRD and SEM techniques. Effects of various reaction parameters towards the reaction performance were studied. The performance of the catalyst was tested based on nature of the catalyst (honeycomb coated or powder form), reaction time (1 to 5 h), molar ratio (1:1 to 1:12 levulinic acid to ethanol) and reusability of the catalytic material. An excellent yield (86-88 %) of ethyl levulinate was obtained under optimized conditions. An attempt is made to correlate the activity of the catalysts in this esterification reaction with their surface characteristics. The honeycomb monoliths coated with zirconia and its modified forms were found to be ecofriendly, cost-effective and reusable catalytic materials compared to their powder forms

2009-2014

Authors: Rakesh Kumar and Varinder Sahni

Present study was carried out to investigate the mechanical properties of newly developed cast aluminum alloy with addition of copper 1.0 % (at.) and magnesium 1.0 % (at.) in the mole ratio of 1:1:1 Al-Cu-Mg. The selection of Cu-Mg on the basis of stoichiometric calculations, 0.55 (at. %) of copper and 0.21 (at. %) of magnesium were mixed in liquid aluminium base material, which was prepared in electric furnace. The melt was held at 750 ºC with alloying additions of copper and magnesium for about 5 min to ensure complete homogenization. Further, this liquidous aluminium metal matrix was stirred at 500 rpm for 5 min and poured at 700 ± 10 ºC in permanent mild steel mould at 200 ºC in order to achieve as-cast alloy. Solution treatment at 500 ºC for 1 h and thermally aged at temperature 160 ºC for 5 h was exposed. The effect of solution and thermal aging temperature on metallurgical morphology and the role of intermetallic compounds on mechanical properties of as-cast alloy have been studied. The optical microscopy and scanning electron microscopy equipped with energy dispersive spectroscopy were used to identify the intermetallic phases and formation of different precipitates was studied by using X-ray diffraction. The improvement in ultimate tensile strength and hardness values have been reported.

2022-2028

Authors: Aravind Rudrarapu , Gouri Sankhar Brahma and Suprava Nayak

A new octahedral cobalt(III) complex of 1,5-bis(2-hydroxybenzamido)-3-aza pentane was synthesized and characterized by elemental analysis, UV-visible, IR, mass spectrometry and thermal analysis methods. Oxidative behaviour of the complex towards the physiologically abundant tripeptide, glutathione(GSH) was studied by UV-visible and FT-NMR techniques. Kinetics of electron transfer between the complex and GSH was studied at 25.0 ≤ t/°C ≤ 45.0, 0.025 ≤ [H+ ]/mol dm-3 ≤ 0.20 and I = 1.0 mol dm-3 (NaClO4). NMR spectra of the reaction mixture were taken as a function of time. Changes observed in the NMR-spectrum during the period of scanning are the initial disappearance of the fine structure and subsequent broadening of the signals of GSH protons. Peaks at (δ, ppm): 2.93 and 2.98, characteristics of Cys-CH2 δ protons in GSH get disappear slowly and new peaks develop at (δ, ppm): 3.33 and 3.38, corresponding to resonating frequencies of Cys-CH2 δ protons in GSSG. Likewise, the peak at (δ, ppm):2.93, characteristic of Cys-CH2 δ proton in GSH is replaced by the resurgence of two peaks at (δ, ppm): 4.3 and 4.1 ppm, commensurate with the resonating frequencies of same set of protons as that of GSH but in a dimeric environment. The time dependent NMR simulation of the reaction reveals that GSH reduces the CoIII moiety successfully, while it gets converted into the dimer, GSSG. The relatively fast transformation of GSH to GSSG as evident from both electronic spectra and NMR studies together with the activation parameters obtained from the temperature dependence of reaction rate suggest that there is no involvement of any bridging group for electron transfer and the redox process may be taking place via outer sphere mechanism

2042-2046

Authors: L.V. Ramana1 , M. Suri Appa Rao1 , K.M. Ch. Apparao2,* and B. Nageswara Rao1

A new phenylpropanoid containing flavon-3-ol has been isolated from the leaves of traditional medicinal plant, Walsura trifoliata. The structure of the compound was established on the basis of spectroscopic evidence [2D NMR, HREIMS] and by its alternative synthesis. The synthesis of this natural product was achieved from inexpensive and readily available starting materials of phloroglucinol dihydrate. Key reaction sequence includes Grubbs-II RCM reaction, Wittig reaction and sharpless dihydroxylation using AD-mix α.

2057-2064

Authors: S.R. Ashok1 , M.K. Shivananda1,* and A. Manikandan

Molecular adaptation of small molecules that are targeted as therapeutic agents is a most anticipated one in drug designing and development. In the present approach, a family of substituted 1H-benzo[d]imidazol-2-amine derivatives (5a-d and 6a-e) were effectively synthesised and testified for their molecular adaptations in order to develop them as novel medications against oxidation, inflammation and inflammation associated cancer types by means of in silico and in vitro assessments. Chronic inflammation, regardless of infectious agents, plays a vital role in various cancer development. Moreover, hypoxia-inflammation-cancer are highly associated together. Hydrogen peroxide free-radical scavenging, HRBC membrane stabilization assay and cell viability test by MTT assay (macrophage) were executed to establish antioxidant, anti-inflammatory and anticancer properties of these compounds. As the prostaglandin-endoperoxide synthase 2 is highly involved in inflammation and cancer development respectively, molecular docking was executed on the corresponding X-ray crystallographic models (PDB structures).

2069-2072

Authors: A. Damodara Reddy1,* and M.L.S. Deva Kumar2

In the proposed research article, polymer nanocomposites on the basis of thermoset polymer resultant blends (epoxy/polyester) having wollastonite powder are prepared by high shear mixer (mechanical), followed by an ultra-sonicator for uniform dispersion of wollastonite particulates in the final blend matrix. Wide range percentages of modified wollastonite nano-particulates with 0, 1, 2, 3, 4 and 5 wt. % were incorporated into the epoxy/polyester blend matrix in order to evaluate the effect of nanofillers on nanophase morphological structure and to study material properties. Various thermal parameters of the nanocomposite were evaluated using thermogravimetric analysis and differential scanning calorimetry techniques. Further, the scanning electron microscopy images have been employed to know fractured surfaces of the titled compound. From the experimental data it was found that uniform miscibility of epoxy/polyester blend mix and homogenous dispersion of wollastonite nano particulates in the blend matrix was noticed. From the TGA studies, 8 % weight loss and 4 °C rise in decomposition temperature was observed with addition of 5 wt. % wollastonite when compared with the 0 wt. % wollastonite combination of epoxy/unsaturated polyester resin blend. DSC results further revealed that the modified wollastonite nanoparticles is major responsible for the glass transition temperature (Tg) of the nanocomposites.

2083-2086

Authors: Nurhaeni1,*, Ahmad Ridhay1 and A.H. Laenggeng2

Snails fields (Pilla ampulaceae) have a hard shell and are known to be one of the sources of biomaterial called chitin. Chitosan is a natural biopolymer that can be obtained from chitin deacetylation. The objective of this study was to obtain the optimum conditions of chitin deacetylation in highest degree deacetylation of chitosan. This study used random complete method that contains various of NaOH concentration (30, 40, 50, 60 and 70 %), temperature of deacetylation (60, 90, 120, 150 and 180 °C), time of deacetylation (1, 2, 3, 4 and 5 h) and ratio between NaOH and chitin (1:4, 1:6, 1:8, 1:10 and 1:12 b/v) with three repetitions. The deacetylation degrees of chitosan were determined by FTIR. The results show the optimum condition of deacetylation degrees of NaOH concentration, temperature, time and ratio of NaOH and chitin are 60 %, 150 °C, 4 h and 1:10, respectively. This produces the highest deacetylation degree of chitosan rate of 83.23 %.

2091-2094

Authors: R. Djarot Sugiarso K.S, Arum Dwi Kurnia, Dewi Ratnawati, Haryudini Arsa Putri, Herdayanto S. Putro and Ratna Ediati

This study aims to investigate the optimum conditions of five reducing agents viz., sodium thiosulfate (Na2S2O3), hydroxylamine hydrochloride (NH2OH·HCl), ascorbic acid (C6H8O6), sodium oxalate (Na2C2O4) and sodium sulfite (Na2SO3) for the reduction of Fe(III) to Fe(II) using UV-Vis spectrometry. As result, the optimum pH of acetate buffer for Na2S2O3, NH2OH·HCl, C6H8O6, Na2C2O4 and Na2SO3 were obtained at pH 4.5, 4.5, 4.5, 5.0 and 4.0, respectively. Whilst the optimum time for each Na2S2O3, NH2OH·HCl and C6H8O6 were 15 min, the outcome for Na2C2O4 and Na2SO3 took longer time which are 45 and 30 min, respectively. As for optimum concentration, the results were various as Na2S2O3, NH2OH·HCl, C6H8O6, Na2C2O4 and Na2SO3 were at 11, 7, 5, 12 and 60 ppm in consecutive order. Also to conclude the work, the recovery percentage were calculated and the results were Na2S2O3 (102.81 %), NH2OH·HCl (116.71 %), C6H8O6 (97.97 %), Na2C2O4 (85.89 %), and Na2SO3 (85.04 %).

2101-2106

Authors: A.F. Mazlan, S.H. Loh and W.M.A.W.M. Khalik

This study report the optimal condition of an extraction method for caffeine residue analysis in water. C18 was impregnated with cellulose triacetate by using a solution casting method to produce a thin film. Optimization work was performed based on a 23-full factorial central composite design, which was subjected to salt addition, extraction time, and stirring rate as the main parameters. The optimum condition suggested by the model was as follows; salt addition (0.6 %, m/v), extraction time (11 min) and stirring rate (300 rpm). The generated model and 2-way interaction were significant at p < 0.05. Detection and quantification limits of the developed method were calculated at 0.06 and 0.21 ng/mL, respectively. The thin film displayed exceptional recovery (83.90-98.50 %) and repeatability (7.71-12.40 % RSD) at two levels of concentration.

2111-2115

Authors: Raghad Ali Hamed, Sabreen Shaker Mahmood and Ban Dawood Salih

In this article, a series of Schiff-base compounds is prepared by consending aromatic dialdehydes and diamines in the presence of p-toluenesulfonic acid as catalyst. The prepared Schiff bases are characterized by CHNS/O, NMR and FTIR techniques. Moreover, analytical applications of Schiff bases as chelating agent was evaluated by loading (20 %) of compounds (B and C) the urethanic foams. Furthermore, chelating resins type P1 (B) and P2 (C) are also prepared by loading the Schiff base into polymer backbones. Moreover, the batch process is used to study the ability of these resins in recovering metals ions, such as (Mg2+, Pb2+, Cu2+, Cr3+, Ni2+, Co2+, Cd2+ and Ca2+). The study is performed by considering the contact time and pH value. Finally, the polymer’s maximum loading capacity is in the following sequence: P1 (B) Co2+ > Cr3+ > Mg2+ > Ni2+ > Cd2+ > Ca2+ > Pb2+ > Cu2+; P2 (C) Mg2+ > Cd2+ > Ca2+ > Co2+ > Pb2+ > Cu2+ > Cr3+.

2121-2124

Authors: Yi Yang, Xia Tong, Gen Luo, Yumei Shu and Yubing Zheng

We report herein the synthesis of CuSCF3 complex supported by 6,6′-dimethyl-2,2′-bipyridine via the strategy of triphenylphosphine-mediated deoxygenation of CF3SO2Na in the presence of cuprous chloride. The molecular structure of this new cuprous complex was characterized by elemental analysis, 1H (13C, 19F) NMR spectra and verified by X-ray crystallography. Unlike the classical [(2,2′- bipyridine)Cu(SCF3)] complex, 6,6′-dimethyl-2,2′-bipyridine supported cuprous trifluoromethylthiolate complex was dimerized in the form of [{(6,6′-dimethyl-2,2′-bipyridine)Cu(SCF3)}2]. The X-ray crystal structure revealed the Cu2S2 cyclic pattern and sulfur atoms serving as the bridge. The Cu-Cu distance was equal to 3.083 Å which was remarkably longer than the analogous [{(1,10-phenanthroline)Cu(SCF3)}2] (2.5781(9) Å). This interesting phenomenon demonstrated that the substituents on the ligand scaffolds have profound influence on the coordination modes of these N,N-ligand coordinated CuSCF3 complexes

2133-2138

Authors: V.M. Boitsov1,2,*, N.A. Knyazev1,3, S.V. Shmakov, S.Yu. Vyazmin, D.M. Nikolaev1, O.B. Chakchir1 and A.V. Stepakov4,5

Benzo[h]isoquinoline scaffold is of interest as a rigid subunit that can be useful for constructing biologically active products. However, no good-yielded synthetic pathway to this ring system has been reported yet. Herein, a facile one-pot synthesis from N-aryl itaconimides and 1,3-diarylisobenzofuran via strong acid triggered skeletal rearrangement reaction is described. Theoretical study for this rearrangement is provided at M11/cc-pVDZ level of theory. Antitumor activity of obtained benzo[h]isoquinoline derivatives against human erythroleukemia K562 cell line was evaluated in vitro by MTS-assay.