Asian Journal of Chemistry

982-986

Authors: Muhammad Yusuf* , Dahniar, Destria Roza and Marini Damanik

ab initio method used on the mechanism of acetalization of 2-methoxybenzaldehyde. ab initio method is a quantum mechanical approximate calculation and derived directly only from theoretical principles. All geometry optimizations were performed using 3-21G and 6-31G* basis set with Hyperchem 8.0 software (windows version). The aim of this study was to focus on the study of the mechanism of acetalization of 2-methoxybenzaldehyde using hydrochloric acid as catalysts. The computational calculation not only provided possible reaction steps but also provided possible energy change in each step of the reaction mechanism of acetalization of 2-methoxybenzaldehyde. The result showed that 2-methoxybenzaldehyde (0 kJ/mol) has the lowest energy and electronegativity compared to acetal product (-17.43 kJ/mol) and a labile hemiacetal (448.33 kJ/mol) due to its stability and the influence of neighbour atom

993-996

Authors: Sanjay S. Kotalwar, Amol D. Kale , Ram B. Kohire and Vasant B. Jagrut *

An efficient and eco-friendly synthesis of 1,5-benzothiazepines has been developed by the reaction of various 2-propen-1-ones with 2-aminothiophenol using microwave irradiation in greener reaction medium, glycerol. The clean reaction conditions, shorter reaction time, high yields and non-toxic, biodegradable reaction medium manufactured from renewable sources are unique features of this method.

1002-1008

Authors: Somana Siva Prasad , G.V. Krishna Mohan*, and A. Naga Babu

A novel reversed-phase high performance liquid chromatographic (HPLC) technique for the determination of everolimus (Isomer-B) and its impurities in the tablet dosage form has been optimized using analytical quality by design (QbD) approach. All the compounds are monitored with the photodiode array (PDA) detector at 280 nm and the parameters namely; precision, accuracy, specificity, stability, linearity, limit of quantitation (LOQ) and limit of detection (LOD) are evaluated. The quantitation limits of IMP-A, IMP-B, IMP-C, IMP-D, IMP-E, Sirolimus and TGR are found to be 0.08, 0.08, 0.10, 0.10, 0.10, 0.08 and 0.08, respectively. Recovery studies from 0.9 mg/L to 9.0 mg/L are performed for all impurities and the values were obtained between 85-110 %. Injection volume and test concentrations have been optimized to achieve LOQ values under the reporting threshold. The whole technique is developed and validated as per International Council for Harmonization (ICH) guidelines. The proposed method is robust, sensitive, rapid and successful and helpful in the regions where regulatory agencies recommend HPLC analytical method

1013-1016

Authors: J.B. Veeramalini* , B. Bharathiraja, S. Raghu Vinayak, R. Vignesh and S.K. Raghul

In present work, water treatment processes is carried out by an affordable, readily usable and non-chemical method. This study involved the process of water may reduce the concentration of particulate matter that includes suspended particles, micro organisms, a range of dissolved and particulate material derived from the surfaces. The substances used in this work were coarsely blended with each other and a special composite fibre filter was made. Several processes variables of quality of waste are also measured before and after the treatment. Results show that the water quality has been enriched in several ways such as reduction in the dissolved solids, pH has been controlled, deodorization and prevention of microbial growth. Hence use of this work has been utilized as a “Homemaker Model” and act as an alternative method for wastewater treatment in a cost effective way.

1022-1026

Authors: Nour Abd Alrazzak , Suad T. Saad and Nagham Mahmood Aljamali *

In the present study, new heterocyclic organic ligands were synthesized using amoxil drug as a starting material through multi steps. The ligands were prepared through condensation reaction to form thiazole and imidazole derivatives containing azo or anil groups in their structures via azotization reaction and imination reaction. The new ligands of amoxil have been characterized by means of spectral (IR and 1 H NMR) and thermal analyses

1034-1040

Authors: Roberto García-Monroy , Francisco Prieto-García*, William Scott-Monks , Griselda Pulido-Flores and Judith Prieto-Méndez

To determine levels of metal bioaccumulation (Cd, Cr, Pb and Al) in weaves and corporal fluids of the inhabitants of Xochitlán, Hidalgo, has been the objective of this study. With a view to realising valuations of risk and probable damages to the health of its settlers, the study with a sociodemographic characterization began, with settlers between 6 and 90 years of age. As exclusion criterion were considered, congenital malformations, immunosuppressive sufferings and less than five years of residence in the locality. An inverted population pyramid appeared; of a total of 1947 inhabitants, the population between 10 and 19 years occupies the center of the pyramid, that thins in the ends of the life (5> X> 60 years). A methodology, combined with the established by the ATSDR and the EPA has seted out and adding an instrument of survey (clinical anamnesis) for the characterization of individuals and populations with ample clinical approach. Of the interrelation of flowed and woven metal concentrations in, with aspects of environmental risks it will be possible to be poured off a present, retrospective situational diagnosis and a vision to future, on the behaviour of the contamination and its impact in health factors. The evaluated metal bioaccumulation was present in all the fluids and weaves of the settlers selected between 6 and 90 years of age. One has been a probable relation between these results and those of previous studies of metal accumulation in waters, grounds and cultures

1045-1048

Authors: Quang Thuong Tran*, Loan Thi Thanh Vu , Tram Huyen Le , Ly Thi Phuong Giang and Toyonobu Usuki *

The objective of this study was to evaluate the effects of extraction parameters (ethanol concentration, extraction ratio of solvent to raw material and extraction time) on the yield of spinosin from the seeds of Ziziphus mauritiana Lam. Box-Behnken factorial design was used in association with response surface methodology. The optimal extraction conditions were an ethanol concentration of 61 %, 40 (v/w) liquid-to-solid ratio, and 2.6 h extraction time with reflux. Spinosin was purified using Diaion HP20SS as an adsorbent. The maximum spinosin yield was 1.18 mg/g raw material. Present findings can be applied to future approaches for maximizing the extraction of spinosin from Z. mauritiana Lam. seeds.

1057-1061

Authors: R. Nagarajan and L. Emmanuvel*

In this communication, the authors described the synthesis of 1-arylamino-1,2,3-triazole derivatives via diazo transfer reaction on active methylene hydrazones. Further, we have observed the reduction of 1-arylamino-1,2,3-triazole using Pd/C, H2 to result in unusual N-N bond cleavage to give 4,5-disubstituted-1H-1,2,3-triazole.

1071-1076

Authors: Rajvir Kaur*, and Harpreet Kaur

In the present work the efficiency of activated carbon made from stems of Ricinus communis (CRC) has been studied for removal of anionic dye- Amido black 10B from aqueous solution. The adsorbent has been characterized with scanning electron microscopy (SEM) and Fourier transformer infrared (FT-IR). The effects of various experimental parameters such as contact time, adsorbent dose, initial dye concentrations, pH, concentration of salt and temperature have been studied. Langmuir, Freundlich and Tempkin isotherm models have been used for describing the adsorption process. Of these, Langmuir isotherm model has best fitted the experimental data with a maximum adsorption capacity of 7.12 mg/g. Kinetics studies indicate that the adsorption of Amido black 10B has favoured toward pseudo-second-order model with high correlation coefficients. Thermodynamics parameters confirmed that the adsorption has been found to be spontaneous and endothermic in nature. These results suggested that CRC has a potential low-cost adsorbent for the removal of toxic dye Amido black 10B.

1081-1086

Authors: P.R. Ghutepatil , A.B. Salunkhe , V.M. Khot , B.R. Thombare and S.H. Pawar*

Biocompatible magnetic nanoparticles with enhanced heating proficiency are required for magnetic hyperthermia in order to use it efficiently in cancer treatment. In this paper, ethylenediamine functionalized monodispersed manganese iron oxide (MnFe2O4) nanoparticles were synthesized by using polyol method and functionalized nanoparticles were characterized by using X-ray diffraction, scanning electron microscope, transmission electron microscopy, vibrating sample magnetometry, fourier transform infrared spectroscopy and thermogravimetric analysis techniques for structural, morphological and magnetic analysis. Hyperthermia characteristics of functionalized MnFe2O4 nanoparticles were studied at 167.6, 251.4 and 335.2 Oe to assess the feasibility magnetic hyperthermia anticancer therapy. Outcome revealed that nanoparticles the self-heating temperature rise up to 48.76 to 56.34 °C at 5 and 10 mg mL-1 concentrations in water respectively. Specific absorption rate 94.65 W g-1 was observed at 5 mg mL-1 concentration. Biocompatibility study of functionalized nanoparticles has divulged almost no toxicity for nanoparticles

1091-1094

Authors: R. Kishore , M. Kamboj,*, , M. Shukla, and N. Srivastava

A simple, rapid and green methodology to synthesize cyclic dithiocarbamates (compounds 1-9) was developed by the reaction of 1° amines, CS2 and ethyl 3-bromo-2-oxopropanoate (ethyl bromopyruvate) facilitated by Triton-B as phase transfer catalyst. These compounds (1-9) were characterized with the help of elemental analysis, IR, NMR and mass spectroscopic methods This efficient green approach requires mild conditions and gives good yield of product. In vitro antimicrobial activities of these compounds are reported against the pathogenic bacteria and fungi.

1100-1104

Authors: Jayashri N. Nair , Y.V.V. Satyanarayanamurthy* , N.S.C. Chaitanya and M. Ramesh

The objective of the present work was to develop a heterogeneous base catalyst K2CO3/ZnO for transesterification of algae oil. This catalyst was prepared by wet impregnation method calcinated at high temperature of 600 °C. The catalyst was characterized by X-ray diffraction technique. The crude algae oil was degummed and its free fatty acid was reduced to 2 % by methanol treatment. Methanol was used to convert triglycerides to biodiesel using K2CO3/ZnO. The doping of 30 % K2CO3 on ZnO calcined at 600 °C was studied on biodiesel yield. The reaction parameters such as temperature, stirring rate, amount of catalyst, methanol to oil molar ratio on the yield of fatty acid methyl ester were investigated. Highest yield was obtained for 7 % catalyst, 9:1 methanol to molar ratio at 80 °C for 30 % K2CO3/ZnO. This study proved that the catalyst loading less than 5 % was unsuccessful in biodiesel yield. The physio-chemical properties of the produced algae biodiesel was determined as per ASTM test procedures.

1110-1112

Authors: O. Politeo*, and I. Ercegovic

The volatile oil from leaves of Arbutus unedo L. from Croatia was subjected to chemical composition and acetylcholinesterase inhibition activity. The tested volatile oil was dominated by nonterpene compounds, with (E)-2-decenal, nonanal, nonanoic acid and octanol as main compounds. Terpene compounds were identified in lower quantity, with linalool and α-terpineol as main ones. Results showed low to moderate acetylcholinesterase (AChE) inhibition potential of tested oil, for tested concentration of 1 mg/mL.

1128-1132

Authors: P.P. Badoni1 , Goutam Kumar *, Mahender Singh , Navneet Singh , Arun K. Khajuria , Bharti and Sanjay Dutt

In present study, the Geranium wallichianum leaf extract (aqueous) and 1 mM silver nitrate solution (aqueous) were amalgamated to synthesize silver particles within the nanometer range. Initial colour changes and surface-plasmon-resonance (SPR) absorbance band observed in UV-visible spectroscopic study gave support to configuration of silver nano-particles. Silver nanoparticles were characterized by XRD, TEM and FTIR spectroscopy. Then antimicrobial (antibacterial and antifungal) activities of silver nanoparticles against selected microbial strains were studied by well diffusion method. During this work, silver SPR absorption bands between 405-425 nm range were shown by Geranium wallichianum leaf extract mediated synthesized silver nanoparticles sample solutions at different intervals. X-ray diffraction pattern displayed the formation of face centred cubic phase silver nano-structures. TEM measurements confirmed that silver nanoparticles are spherically shaped and maximum particles in 9-16 nm size range having average diameter 12.5 nm. Important FT-IR peaks at 3314.11, 1710.60, 1587.11 and 1347.77 cm-1 were predicted for hydroxyl, carbonyls, unsaturated C-C bonds and phenolic groups respectively. Further from antimicrobial results, it has been found that values of diameter of zone of inhibition (mm) of synthesized silver nanoparticles against B. subtilis, S. aureus, L. plantarum, P. aeruginosa, A. niger and C. albicans strains were 32, 28, 25, 25 35 and not active, respectively. MIC-MLC (µL) values were also determined. At last, it can be concluded that antimicrobial agents of 9-16 nm size range and stabilized by polyhydroxy-bioactive-components present in extract, in the form of silver nanoparticles has been productively synthesized.

1137-1142

Authors: Sunil B. Shinde* and Raj M. Deshpande

Hydrogenation of aromatic dicarboxylic acids gave 100 % selectivity to respective cyclohexane dicarboxylic acid with 5 % Pd/C catalyst. 5 % Ru/C catalyst was observed to give over hydrogenation products at 493 K and at lower temperature (453 K) the selectivity for cyclohexane dicarboxylic acids was increased. Hydrogenation of phthalic acid with Ru-Sn/Al2O3 catalyst was observed to give phthalide instead of 1,2-benzene dimethanol or 2-hydroxy methyl benzoic acid. Ru-Sn/Al2O3 catalyst selectively hydrogenated the carboxylic group of cyclohexane dicarboxylic acids to give cyclohexane dimethanol. Use of proper catalysts and reaction conditions resulted in desired products.

1149-1152

Authors: Mohammed Mujbel Hasson*, , Basim H. Al-Zaidi and Ahmad H. Ismail

Two new unsymmetrical imidazolium salts viz., [1-(4-ethylphenyl)-3-propyl-1H-imidazole-3-ium bromide] (3) and [1-(2,6-dimethylphenyl)-3-propyl-1H-imidazole-3-ium bromide] (4) have been synthesized via the reaction of propyl bromide with imidazole derivatives, [1-(4-ethylphenyl)-1Himidazole] (1) and [1-(2,6-dimethylphenyl)-1H-imidazole] (2) in absence of solvent. Then two new N-heterocyclic carbene silver complexes (5 and 6) were prepared through the reaction of imidazoluim salts (3 and 4) as a source of N-heterocyclic carbene with Ag2O by in situ method. These complexes can be used in the future as a transfer agent for preparing other transitional metal carbine complexes (NHCs) via transmetallation method. The formation of these compounds was confirmed by spectral analysis.

1158-1162

Authors: R. Anitha , E. Kumar,*, and S.C. Vella Durai

This paper explains the details on the preparation of polyaniline/CeO2 (10 wt %) nanocomposites using the method of in situ polymerization. The formation of PANI/CeO2 nanocomposites were proposed via oxidation of aniline and reduction of CeO2, respectively. The effect of CeO2 concentration on AC conductivity, morphological, optical and structural properties of the prepared PANI/CeO2 nanocomposites material were examined. The structural studies show the presence of CeO2 nanoparticles were occurred in PANI of nanocomposites. The average grain size of PANI/CeO2 nanocomposites varied with increasing and decreasing concentration due to the process of nucleation during the polymerization. The average particle grain sizes were measured from HRTEM. The morphology analysis was carried out from SEM. The UV absorption spectrum showed that the absorption peak of CeO2 nanoparticle at 341 nm, shifted to lower wavelength side, the nanocomposite absorption peaks at about 324, 368 and 858 nm was confirmed by the formation of PANI/CeO2 nanocomposites. The electronic structure of the band gap of the nanocomposite materials were calculated using ultraviolet visible absorption spectrum. The band gap energy of nanocomposite is 3.36 eV. The FTIR spectrum clearly showed the strong presence of CeO2 nanoparticles in PANI chain. The AC conductivity varied with varying the temperature and depends on the concentration due to the formation of PANI/CeO2 nanocomposite.

1169-1175

Authors: S. Sivakumar, S. Rameshkumar , S. Sathishkumar and A. Sankar

Artificial planar bilayer phospholipid membrane was formed in KCl bath solutions and its electrical properties have been analyzed using electrochemical impedance spectroscopy. The stability of planar bilayer lipid membrane depends on concentration of KCl in the bath. Changes in the electrical properties of planar bilayer lipid membrane with the addition of lorazepam were also studied using electrochemical impedance spectroscopy. Lorazepam gets partitioned into bilayer lipid membrane and exhibited a fluidization effect. The ionic conductance across the bilayer lipid membrane increased with the addition of lorazepam to the bath. An impedimetric sensor was developed for quantification of lorazepam in solution

1181-1188

Authors: S. Gurulakshmi , S. Madeswaran*, S. Karthikeyan and V. Porchezhiyan

In the present study, polymer electrolyte with poly(vinyl alcohol) (PVA) blended with cellulose acetate (CA) was chosen to prepare composite electrolyte using ammonium triflate salt and nano sized alumina (Al2O3- < 50 nm) by the solution casting method. The as prepared samples were characterized by X-ray diffraction, FT-IR, differential scanning calorimetry and AC impedance spectra. The loss tangent and dielectric studies were carried out for all the prepared samples using AC impedance analysis. Activation energy with regression values and relaxation time were calculated and found to be low for the highest conducting membranes. The presence of 0.1 mol content of nano alumina has enhanced the ionic conductivity significantly to the value of 2.012 × 10-3 S/cm from that of the filler-free electrolyte (2.93 × 10-4 S/cm). Ionic transference number was calculated by electrostatic polarization method and it was found to be 0.9684, which shows the conducting species were ions. A proton battery fabricated using the configuration Zn+ZnSO4. H2O || PVA-CA-0.5 mol NH4CF3SO3-0.1 mol Al2O3 || PbO2 + V2O5 produced a steady state open circuit voltage of 1.39 V, which proves the prepared composite electrolyte is suitable solid electrolyte for electrochemical devices.