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Mediterranean Journal of Chemistry

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1 The determination of the folic acid and its selected derivatives, Barbara Krawczyk*, Dominik Szczukocki, Justyna Stachniuk, Rados?aw Da?kowski, Marek Zieli?ski, Renata Juszczak, Ewa Mi?ko? and Robert Zakrzewski
Folic acid (FA) belongs to vitamins from group B. The most commonly used drug from a group of structural analogues of FA is methotrexate (MTX), showing antiproliferatative properties. Unfortunately, the action of MTX is not selective. Toxic effects of methotrexate may be partially abolished by the use of leucovorin (calcium salt of folinic acid, FNA) in conserving therapy. The aim of the presented paper was to develop a new analytical procedure using the capillary electrophoresis, allowing the separation and the quantitative marking of the folic acid, methotrexate and calcium salt of folinic acid. Optimal conditions for the electrophoretic separation were obtained for the following parameters: buffer - 25 mmol/L Na2B4O7,pH 9,76; voltage -30 kV, measurement temperature -30 C, the introduction of a sample to the capillary-hydrodynamically 6 s (0,5 psi). These parameters allowed to obtain LOD 0,6 M for FA, 0,65 M for FNA and 0,7 M for MTX.
2 The study of separation of delaprils s-cis/s-trans isomers and development and validation of an analytical method for the estimation of delapril by reversed-phase liquid chromatography, Afef Ben Amar*, Mbarek Abidi and Najib Ben Hamida
Delapril is an angiotensin converting enzyme (ACE) inhibitor, which exists as a mixture of rotational s-trans and s-cis isomers due to the rotation of the amide bond. Although these stereoisomers do interconvert by rotation about the amide bond, the rate of interconversion is slow, allowing separation of the isomers on the chromatographic time scale. The effect of the flow-rate, column temperature, pH, organic modifier, and counter-ion on the peak shape and the separation of the s-cis and s-trans conformers of delapril was investigated by HPLC. It was proved that the separation selectivity was improved by either a decrease of the flow-rate or an increase of the amount of the organic modifier or the addition of a positively charged counter ion. Delapril was then estimated by a reversed-phase liquid chromatographic method. This method was subsequently validated for specificity, linearity, accuracy and precision, according to the International Conference on Harmonization (ICH) guidelines. An NMR study indicates that the molecule exists as a mixture of rotational cis and trans isomers which confirms the results obtained by HPLC. The isomer ratio integrated from the obtained 1H NMR result was 75:25 in DMSO-d6 at 298 K, where the s-trans isomer was the major form.
3 Density, viscosity and refractive index prediction of binary and ternary mixtures systems of ionic liquid, Gonzalo Astray Dopazo*, Miriam Gonzlez-Temes, Dina Larios Lpez, Juan Carlos Mejuto
Different artificial neural networks architectures were developed to predict the density, viscosity and refractive index of binary and ternary mixtures of ionic liquids using their individual properties. All neural network implemented were evaluated using the root mean square error (RMSE) and the average percentage deviations (APD) for the training and validation phase. The individual models implemented show great values of R2 (greater than 9.995?10-01) and low errors in terms of RMSE, that corresponds with an APD less than 7.766?10-02 %, with the exception of the model for the prediction of viscosity where the error raised to 3.338 %. The results show that the different individual artificial neural networks implemented are a useful tool to predict the density, viscosity and refractive index of binary and ternary mixtures of ionic liquids and with reasonably accuracy.
4 Thermal characterization and comparisons of lignin-formaldehyde and lignin-glyoxal adhesives, Mohamed Ammar*, Ramzi Khiari, Mohamed Naceur Belgacem, Elimame Elaloui
In the present study, the main focus was the use of lignin isolated through an industrial waste (black liquor) to prepare phenolic-type resins. Thermal properties of control lignin-formaldehyde adhesive (RLF) and lignin glyoxal adhesive (RLG) have been investigated in detail. The effect of methylolation of lignin by formaldehyde and glyoxal have been studied using thermogravimetric analysis (TG) and differential scanning calorimetry (DSC). Methylolation has significant effect on the structure and the thermal stability of lignin. Rate of curing is enhanced by the type of curing agent and temperature.
5 Microwave-assisted synthesis of new aryliminothiazolylidene-2-thiazolidin-4-ones and their azarhodacyanines analogues, Souad Kasmi-Mir*, Fatima-Zohra Zradni, Mustapha Rahmouni and Gilbert Kirsch
We here report an efficient microwave-assisted protocol for the synthesis of new arylimino-thiazolylidene-2-thiazolidin-4-ones 6 and their azarhodacyanines derivatives 7 with quantitative yield from 2'-(methylthio)-4'-oxo-3H,4'H-[2,5-bithiazolylidene]-3'-ium tosylates 5 and 2-arylimino-5-(thiazol-2(3H)-ylidene) thiazolidin-4-ones 6, respectively, using as starting material the 4-thiazoline-2-thiones 1 and 3-methyl-2-thioxo-1,3-thiazolidin-4-one 3. The transformation of the tosylate salts 5 into their arylimino derivatives 6 has not been reported to date.
6 Kinetic study by UV Spectrophotometry of Carzol degradation in aqueous medium, Hayet Bakhti* and Najib Ben Hamida
This paper deals with the kinetic hydrolysis in aqueous media of Carzol or (E) 3-dimethylamino- methyleneaminophenyl-N-methylcarbamate hydrochloride. The Carzol is a bifunctional compound which belongs to the chemical families formamidine and carbamate. This work is carried out by UV Spectrophotometry. The successive determination of 3-aminophenyl-N-methylcarbamate and 3-aminophenol, as the mainproducts of the formamidine and the carbamate groups of Carzol hydrolysis gives evidence for the significant reactivity of this insecticide-acaricide in aqueous media. The obtained negative activation entropy ?S? = - 32.39 J mol-1K-1 indicates a BAC2 mechanism involving bimolecular collapse of the formamidine group of Carzol. While, the obtained positive activation entropy ?S? = +100.24J mol-1 K-1and the absence of basic general catalysis indicate an E1cB mechanism involving unimolecular collapse of the carbamate group of Carzol via a methylisocyanate intermediate.
7 Synthesis and antitubercular evaluation of new 1,2,3-triazole derivatives of carbohydrates, Juliana Alves dos Santos, Roberta C. N. Reis Corrales, Fernando R. Pavan, Clarice Queico. F. Leite, Rafael Mafra de Paula Dias and Adilson David da Silva*
We reported in this work the preparation of novel 1,4-disubstituted-1,2,3-triazoles derivatives from D-glucose and D-fructose and their in vitro antibacterial activity against Mycobacterium tuberculosis were evaluated. The chemical synthesis was performed based on the 1,3-dipolar cycloaddition reaction, and antimicrobial activity was determined based on Resazurin Microtiter Assay against Mycobacterium. None of the triazole glycoconjugates tested showed activity against these microorganisms.
8 Study of Chemical Interactions in Binary mixture water-1,4-dioxane: Neighbourhood and Associated Model Approach, Rafik Besbes*, Noureddine Ouerfelli and Manef Abderabba
We use our results of measurements of the activities coefficients of water and 1,4-dioxane at room conditions to analyse the interactions between molecules of water and 1,4-dioxane in different mixtures. Our study is based on Neighbourhood Model Approach at liquid state in correlation with solid state to calculate molar fractions of free molecules of water and of 1,4-dioxane in pure liquid state and to deduce the composition of the various mixtures. We calculate system composition in a basis of associate model (called). This model gives good results to interpreting interactions between molecules of water and of 1,4-dioxane. Our model is inspired by resulting experimental recently published by our team, witch measurements of the enthalpy of mixture: ?mh (XD), present two maxima for molecular fraction of 1,4-dioxane XD = 0.1438 and XD = 0.7805, which correspond to arrangements between molecules of water and 1,4-dioxane of type WD3.56, and DW5.95 (D: 1,4-dioxane W: water) We use, for the study of the model suggested, a number of 4 neighbours molecules in the first shell surrounding one molecule of water and 6 neighbours molecules for one molecule of 1,4-dioxane. Our observations confirm well the results of works of many authors by different technical methods.
9 Highly diastereoselective synthesis of N-substituted 4-(diethoxyphosphoryl)-pyrrolidines-3-carboxylate starting from tetraethyl methylenediphosphonate, Maha Ameur, Acha Arfaoui, Jihne Ben Kraem, Salem S. Al-Deyab and Hassen Amri *
This paper describes a convenient synthesis of novel series of 3,4-disubstituted pyrrolidines based on the aza-Michael addition of primary amines to 3,4-difunctionalized-1,3-diene followed by an intramolecular cyclization.
10 Chemical composition, antibacterial and antioxidant activities of Tunisian garlic (Allium sativum) essential oil and ethanol extract, Raja Zouari Chekki, Ahmed Snoussi, Imen Hamrouni and Nabiha Bouzouita *
The aim of the study is to establish some nutritional properties of garlic cultivated in Tunisia and to evaluate the antioxidant and the antimicrobial activites of its essential oil and ethanol extract. Tunisian garlic (Allium sativum) was characterized for moisture, ash and protein contents which were determined as 66%, 1.4% and 5.2% respectively. In addition, Fe (5.90 mg/kg), Cu (1.61 mg/kg), Mg (15 mg/kg) and P (140 mg/kg) were reported such as the major minerals in garlic. The fat profile of tunisian garlic was conducted, the main fatty acids identified were lauric acid (49.3%) and linoleic acid (20.4%). Essential oil obtained from A. sativum was analysed by capillary GCMS. Diallyl disulfide (49.1%) and diallyl trisulfide (30.38%) were the main components of the five identified components. The phenolic content of the ethanol extract are analysed for its phenolic profiles, colorimetric analysis revealed that the total phenols, flavonoids and proanthocyanidins contents were respectively 43.63 mg GA/g, 13.18 mg quercetin/g and 24.24 mg of catechin/g. Antioxidant activity was evaluated by DPPH (2,2-diphenyl-1-picrylhydrazyl) assay, essential oil presented the highest antioxidant activity compared to its ethanol extract. IC50 values observed for the essential oil and ethanol extract were 300 ?g/ml and 600 ?g/ml respectively. The essential oil and ethanol extract from raw garlic were tested for antimicrobial activity against seven microorganisms. The results showed that ethanol extract was active against all tested strains: Escherichia coli, Salmonella typhi, Staphylococcus aureus, Pseudomonas aeruginosa, Listeria monocytogenes, Yersinia enterocolitica and Bacillus cereus.
11 The synthesis of a glucoconjugate of the peptidic fragment of cryptophycin-24, Abdelmoumen Mezrai, David Lesur, Anne Wadouachi, Florence Pilard and Joseph Kajima Mulengi *
A novel glucoconjugate of the peptidic fragment of cryptophycin-24 was prepared through the replacement of the leucic acid residue with L-leucine and the functionalisation of tyrosine residue with glucose. Those modifications lead to a novel protected tripeptide fragment of cryptophycin-24.
12 Kinetics of the photoinduced dissociative reduction of the model alkyl peroxides di-tert-butyl peroxide and ascaridole, David C. Magri* and Mark. S. Workentin
Rate constants for the reaction between excited singlet state aromatic donors and the dialkyl peroxide, di-tert-butyl peroxide (DTBP), and the bicyclic endoperoxide, ascaridole (ASC), were measured in acetonitrile using fluorescence quenching techniques. The rate constants, measured with 18 different aromatic donors by Stern-Volmer quenching, range from 9.2 ? 109 to 4.4 ? 106 M-1 s-1. Using accurately measured standard reduction potentials for the peroxides, the driving force for photoinduced electron transfer is predicted to be thermodynamically feasible over the entire range of excited donors ranging from ?49 to ?10 kcal mol-1 for ASC and ?38 to ?2 kcal mol-1 for DTBP. However, when the photoinduced kinetics are combined with previously measured electron transfer kinetics by homogeneous redox catalysis with ground state radical-anion donors, a smooth parabolic correlation for a dissociative electron transfer mechanism is not observed. Rather, a discontinuity is observed between the photochemical and electrochemical data sets with the rate constants with singlet excited states donors being over two orders of magnitude larger than the ground state kinetics at the same driving force. The discrepancy is examined considering the importance of attractive interaction between fragments in the dissociative photoinduced electron transfer reactions.
13 Selective Release of antiTB Drugs Complex from Smart Copolymeric Bioactive nanocarriers, Alejandro ArredondoPearanda, Luis Guillermo GuerreroRamrez, Maria Dolores Blanco Gaitn, Eduardo Mendizbal and Issa Katime*
Smart nanocopolymeric matrices have been employed to load and release anti tuberculosis (anti TB) drugs combinated complexes of Ethambutol (EMB), Isoniazid (INH), Rifampicin (RMP) and Pyrazinamide (PZA). Copolymeric nanocarriers were synthesized using a microemulsion polymerization method previously reported. These nanocarriers can show selective swellingcollapse response under changes in local environments such a temperature, pH, solvent composition and electrical stimuli. The employ of these kinds of systems permits a controlled and selective delivery and release on specific human tissues. High Performance Liquid Chromatography technique was used to allow the detection of combinated mixtures of different active principles of antiTB drugs using an acetonitrile mobile phase at 0.5 mL/min of flow rate whit a Spherisorb ODS2, C18 column. The results obtained suggest that the employ of smart nanohydrogels is a novel method in several tuberculosis therapies.
14 Anion exchange removal of Al3+ from Li+-Al3+ aqueous solution (originating from lithium recovery from brine), Anissa Somrani *, Ahmed Hichem Hamzaoui and Adel MNif
The purpose of this study is to separate aluminum(III) ion from an aqueous solution containing Li+ at 25C. Al3+ was transferred into [Al(C2O4)3]3- by means of complexation and removed by an anion exchange resin. This resin was anionic type Amberlite IRA 402 regenerated by sodium chloride. Hence, a theoretical study based on speciation diagrams was carried out to determine the best pH domain for separation. The complexation of aluminum ions by ammonium oxalate was studied. The motar ratio of Ox/Al and pH was investigated. Optimum values of these factors were found to be 3 and 4 respectively. In this case, the remaining lithium is 98.5%.
15 Study of the reaction of (Z)-5-bromo-3-(1-methylpyrrolidin-2-ylidene)-3H-indole with pentane-2,4-dione, Masomeh Aghazadeh, Mehdi M. Baradarani*, Madeleine Helliwell and John A. Joule
The reaction of (Z)-5-bromo-3-(1-methylpyrrolidin-2-ylidene)-3H-indole with refluxing pentane-2,4- dione gave two compounds, the major product, 1-[(E)-4-(5-bromo-1H-indol-3-yl)-1-methyl-2,5,6,7-tetra-hydro-1H-azepin-2-ylidene]propan-2-one being accompanied by 1-(7-(2-amino-5-bromophenyl)-1,4-dimethyl-indolin-5-yl)ethanone. Each product is believed to be derived from initial protonation of (Z)-5-bromo-3-(1- methylpyrrolidin-2-ylidene)-3H-indole by the diketone followed with nucleophilic diketone-C-3- addition at the C-2 of the 3H-indolium cation.
16 Biocidal effects of aqueous extract of the roots of Anacyclus pyrethrum (Asteraceae) on Callosobruchus maculatus (Fab.) (Coleoptera : Bruchidae), Samira Khannouchi, Fatima Elhilali and Touriya Zair*
In Morocco, Callosobruchus maculatus (Fab.) (Coleoptera : Bruchidae) causes very important damage on the seeds of stocked Leguminosae ; its control is carried out exclusively by synthetic insecticides which are harmful for both Man and Environment. Pesticides based on plants constitute an alternative solution in the synthetic insecticides. Many studies have focused on improving forms of using plants that enhance and leverage their insecticidal activity (alcoholic and aqueous extracts, essential oils, etc..). In this study, we sought to evaluate the potentialities of the aqueous extract of the roots of Anacyclus pyrethrum (L.) (Asteraceae) against adults, eggs and the emerging of C. maculatus. The tests were carried out on seeds of Cicer arietinum (L.) (Leguminosae) in the temperature of 28.0 2.0C, photoperiod 12/12 and relating humidity from 70 to 75%. The results obtained showed that the aqueous extract of A. pyrethrum has an interesting insecticide effect against the adults of C. maculatus. It reduced longevity, fecundity, fertility, success rate and it increases the number of non-fertile eggs of these insects, especially for the high doses. This indicates that a durable protection and at low cost against this beetle is possible by using the aqueous extract of A. pyrethrum, which can represent an interesting alternative solution to chemical insecticides.
17 Concentration dependent wetting by aniline-ethanol binary system, Vinjanampaty Madhurima and Jonathan Lalnunsiama
Wetting of five substrates namely glass, indium tin oxide, aluminum oxide, hylam and teflon by aniline-ethanol binary system over the entire concentration range is studied using contact angle measurements. Rapid wetting of the substrates, especially hylam in the aniline rich region is understood in terms of the surface energies of the substrates and the intermolecular interactions between the two moieties. FTIR, dielectric and conformational analysis are used to study the molecular interactions in the binary system.
18 Design of Novel Biosensors for Determination of Phenolic Compounds using Catalyst-Loaded Reduced Graphene Oxide Electrodes, Ondrej Kubesa, Kathleen Morrisey, Samantha Mathews, John Proetta1, Christopher Li, Petr Skladal and Maria Hepel *
Facile and inexpensive method for designing high performance sensors for H2O2 and polyphenols has been developed. The proposed sensors are based on high electrocatalytic activity of Prussian Blue (PB) nanoparticles deposited in situ on high surface area graphene nanosheet-based thin films on a graphite electrode. The exfoliated graphene nanosheets were formed by attaching graphene oxide to the electrode surface followed by their electrochemical reduction to obtain the reduced graphene oxide (rGO), providing high surface area and excellent current-carrying capabilities to the sensory film. The PB catalyst nanoparticles were deposited electrochemically on rGO. This procedure is very time efficient as it reduces the time of sensor preparation from 3 days (according to recent literature) to several hours. The proposed method provides simple means to obtain highly reliable and stable sensory films. The sensor shows a dynamic range of 1500 ?M H2O2 and a rapid response of 5 s to reach 95% of a steady-state response. When combined with immobilized enzymes (horseradish peroxidase or laccase oxidase), it can serve as a biosensor for polyphenols. As the proof of concept, the response of the enzymatic biosensors to polyphenol catechin has been presented delineating different mechanisms of horseradish peroxidase and laccase operation. The proposed sensors are low cost, reliable, and scalable.
19 Amodiaquine analogs. Synthesis and anti-leishmanial activity , Elaine S. Coimbra, Adilson D. da Silva, Rafael M. P. Dias, Roberta C. N. R. Corrales, Marcelle de L. F. Bispo, Carlos R. Kaiser, Marcus V. N. de Souza*
In this work, we report the synthesis and antileishmanial evaluation of 13 amodiaquine (AQ) derivatives (4-aminoquinoline-aryl and 4-quinolinylhydrazones series). The compounds were tested against four Leishmania species and murine macrophages. The appreciable activity of these compounds can be considered an important finding for the rational design of new leads for antileishmania compounds.
20 Perfluoroalkyl Epoxides: Synthesis and Conversion into Ionic Surfactants, Abdelhamid Ayari, Henda Mekni, Najeh Grayaa Jaoued and Ahmed Hedhli*
Perfluoroalkylated surfactants having a quaternary ammonium surrounded by three hydroxyl groups as hydrophilic moiety and a perfluoroalkyl chain as tail were obtained by coupling diethanolamine with perfluoroalkylated epoxide followed by quaternisation. The amphiphilic properties of these surfactants were investigated by measuring their surface and interfacial tensions.
21 Highly stereoselective synthesis of functionalized 1,3-dienes from a new allyl bromide, Asma Fray, Jihne Ben Kraem and Hassen Amri *
New and highly functionalized 1,3-dienes 3 and 4 have been synthesized via two different pathways starting from allyl bromide 1. Firstly, the reaction of allyl bromide 1 with triethylphosphite leads to an allylphosphonate 2, which undergoes the Wittig-Horner reaction with a range of saturated and unsaturated aldehydes gives rise to the corresponding 1,3-dienes 3. Secondly, a highly stereoselective reaction between allyl bromide 1 and nitroalkane salts, offers the possibility to obtaining functionalized (E)-1,3-dienes 4.
22 Ternary cobalt complexes with amino acids: potentiometric study, modelization and solid-state investigation , Schahrazede Aomraoui, Achour Terbouche, Karim Beddar, Safia Djebbar*, Ouassini Benali-Baitich, Gilles Bouet
A study in solution of new ternary complexes of cobalt (II) with the tetradentate ligand Schiff base (N,N-bis (2-hydroxy acetophenone) ethylenediimine; H2L) as primary ligand and the amino acid (histidine or tryptophan) as the secondary one has been realized by potentiometry. The stability constants of the complexes have been determined with the calculation program SIRKO. It has been found that the ternary complexes are more stable than the corresponding binary ones. The study has been completed by modelization of all the species found in solution by molecular mechanics with the program EMO (Energy of Molecule). The complexes isolated in powdered form were characterized by elemental analysis, molar conductance, IR spectra, magnetic and electronic spectra. The spectral results support the binding of H2L with two N and two O donor sites to cobalt ion and the binding of histidine or tryptophan by monodentate maner with O donor site, giving an octahedral geometry. Magnetic and Electronic results show that the Cobalt (II) has been oxidized to Co(III) and has a low spin configuration.
23 Analysis of chemical composition of high viscous oils, Irina Germanovna Yashchenko and Yury Mikhailovich Polishchuk*
The spatial distribution of viscous oils which are considered as an important reserve for oil-production in future were studied on base of information from global database on oil physical and chemical properties. Changes in chemical composition of viscous oils in different basins and continents were analyzed as well. It is shown, on average, viscous oils are sulfur-bearing, low paraffin, highly resinous oils with an average content of asphaltenes and low content of the fraction boiling at 200 ?C. Study results of viscous oils peculiarities of Canada, Russia and Venezuela are given. The analysis results can be used to determine the optimal layouts and conditions of oil transportation, to improve the search methods of geochemical exploration, and to solve other problems in the oil chemistry.
24 Removal of Evans Blue and Yellow thiazole dyes from aqueous solution by Mg-Al-CO3 Layered Double Hydroxides as anion-exchanger, Mohamed Bouraada *, Hassiba Bessaha and Louis Charles de Mnorval
Mg-Al-CO3 Layered double hydroxide (LDH) was prepared by co-precipitation method at constant pH, and subsequently used to remove Evans Blue (EB) and Yellow thiazole (YT) dyes from aqueous solutions. The obtained material was characterized by powder X-ray diffraction (PXRD), Fourier transform infrared spectroscopy (FTIR), thermal analysis and BET. The kinetic and equilibrium aspects of sorption of the anionic dyes from aqueous solution by Mg-Al-CO3 were investigated in batch mode. The sorption kinetic data were found to be consistent with the pseudo-second-order model. Data for YT and EB sorption by Mg-Al-CO3 were fitted better by the Langmuir equation than by the Freundlich equation based on the determination coefficient values R2. The maximum adsorption capacities of 222.2 mgg-1 for Yellow thiazole and 107.5 mgg-1 for Evans blue. The thermodynamic parameters including Gibbs free energy ( ??G), standard enthalpy change ( ??H), and standard entropy change ( ??S) for the process were calculated. The negative ??G value indicates the spontaneity of the removal process.
25 Photoelectrochemical Studies on Inorganic/Organic Aqueous Nano-Suspensions Made by TiO2/poly Neutral Red Assembly, Kasem K. Kasem * and Bell Bennett
An inorganic/organic interface (IOI) consisting of TiO2/polyNeutral Red(PNR) was subjected to photoelectrochemical studies in both aqueous nano-suspensions and in thin solid forms. The effects caused by PNR modifier on the photoelectrochemical behaviour of the IOI were investigated using [Fe(CN)6]4- as a photoactive hydrated electron donor agent. Results show that the adsorption process of [Fe(CN)6]3- (photolysis product) controls the photo-activity outcomes of IOI assemblies. TiO2/PNR shows lower heterogeneous photochemical response than native TiO2 in a short photolysis time. At longer photolysis times the IOI show a photo activity greater than that of native TiO2. TiO2 /PNR nanoparticles adsorb more [Fe(CN)6]3- in a very steady adsorption /desorption process than the unmodified particles. The interface activities were explained by analysing the IOI junction characteristics, such as electron affinity, work function and hole/electron barrier heights. At TiO2/PNR a strong hybridization between electrons-like and hole-like sub band states in close vicinity to the Fermi energy are developed. The aqueous nano-systems retained moderate stability as indicated by the reproducibility of their photo catalytic activities. Both [Fe(CN)6]4- and PNR contributed to the stability of native TiO2 surfaces.
26 Relative Permittivity of Carbon Dioxide + Ethanol Mixtures prediction by means of Artificial Neural Networks, Gonzalo Astray *, Manuel A. Iglesias-Otero, Jorge Morales and Juan C. Mejuto
CO2 + ethanol mixtures have a huge scientific interest and enormous relevance for many industrial processes. Obtaining of their chemical and physical properties is a fundamental task. Relative permittivity (?r) of these mixtures is a key property because allows a better knowledge of the structure and the interactions in other media. In this work predictive values of relative permittivity (?r) of carbon dioxide + ethanol mixtures were obtained implementing artificial neural networks (ANNs). They are used successfully in very different fields; therefore it is a very useful tool. In this case the obtained results enhance the ones from the usual multiple linear regression analysis. In both cases mass fraction, pressure and temperature experimental data from a direct capacitance method were used.
27 3-aminopyridine release study from polymeric supports in homogeneous and heterogeneous media , Hafida Sehil, Zohra Bengharez*, Zineb El Bahri, Houaria Merine and Kaddour Guemra
In order to control and modify the drug release, in one hand 3-aminopyridine as active agent was grafted via chemical azomethine bond on monomer then copolymerized with N-vinylpyrrolidone. The obtained supports were characterized and the drug release from these formulations was followed using UV-Vis spectrophotometer in homogeneous media at four different pH (pH=1.2, 4.0, 6.0 and 8.0) simulating the human digestive rout. The results showed that the hydrolysis of monomer and copolymer obeyed to the first order and the apparent kinetic constants were calculated. In the other hand, spherical dosage forms composed from Eudragit RL100 and the active agent or the copolymer support were prepared and tested to control the drug release. The heterogeneous kinetics were established successively in the four cited media. The drug release seemed that be governed by diffusion model according to the Ficks laws. So, the diffusivities were calculated and the results demonstrated that the drug release can be modified using these formulations.
28 Use of kitchen steel wool as oxygen absorber improves storage retention of beta-carotene in solar-dried vegetables, Hudson Nyambaka*, James Nderitu, Mildred Nawiri and Jane Murungi
Vitamin A deficiency remains a major health concern in developing countries whereas the season availability of vegetables could provide for vitamin A. Dehydration is widely used to preserve dark green leafy vegetables (DGLV) but storage in normal atmosphere condition losses beta-carotene by oxidation, therefore requiring use of an oxygen absorber. The study examined use of kitchen steel wool as an oxygen absorber in reducing the loss of beta-carotene content in three indigenous DGLVs that were solar dried and stored for a period of 168 days in four different packing conditions. Fresh vegetables contained between 781.94 to 1047.42 ?g/g dry matter (DM) beta-carotene, reducing significantly (p=0.01) to between 653.63 to 712.99 ?g/g DM after dehydration. Steel wool oxygen absorber significantly improved (p = 0.02) beta-carotene retention, recording a loss of 19.5 to 37.6% compared to 47 to 72% in normal conditions. Storage of DGLVs under kitchen steel wool oxygen absorber preserves vegetables and retains high levels of beta-carotene.
29 Thermal stability of novel polyurethane adhesives investigated by TGA, Mariusz Mami?ski *, Waldemar Jask?owski and Pawe? Parzuchowski
The objective of the work was an assessment of thermal stability of novel polyurethane wood adhesives by means of TGA. Hyperbranched polyglycerols of various structures were used as polyol components cured with polymeric methylenediphenyldiisocyanate (PMDI) or polymeric hexamethylenediisocyanate (PHDI). Resultant adhesives were thermally degraded in temperature range 20 - 500C. Performance of polyurethane based on fully aliphatic polyglycerol was inferior to those based on polyglycerols bearing aromatic moieties. The differences in 50%-weight loss temperature achieving 27 - 39C as well as residual weights at 480 C indicate the contribution of aromatic units presence within the macromonomer structure to increased thermal stability of polyurethane upon thermal degradation. Furthermore, temperature of 50% weight loss revealed that thermal stability of the developed hyperbranched polyglycerol-based adhesives was comparable to that of the commercial PUR adhesive.
30 Addition of Di(trimethylsilyl) Phosphite to Schiff Bases of 2,5 Diformylfuran, Jaros?aw Lewkowski*, Marek Dzi?gielewski, Aleksandra Szcze?niak and Magdalena Ciecha?ska
A series of 2,5-Furanyl-bis-(aminomethylphosphonic Acids) has been synthesized by the addition of di(trimethylsilyl) phosphite to azomethine bond of achiral Schiff bases derved from 2,5-diformylfuran. The stereochemical aspect of this reaction has been studied and compared with the behaviour of achiral terephthalic Schiff bases in similar reaction. Whereas, addition to achiral terephthalic Schiff bases was found to be highly stereoselective, the analogous reaction with achiral 2,5-diformylfuran Schiff bases was stereoselective exclusively in the case when the substituent is benzyl.
31 Chemical composition, Antimicrobial and anti-acetylcholinesterase activities of essential oils from the Tunisian Asteriscus maritimus (L.) Less, Sined Medimagh, Mejda Daami-Remadi, Hayfa Jabnoun-Khiareddine, Hichem Ben Jannet* and Mhamed Ali Hamza
The chemical composition, the acetylcholinesterase inhibitory effect and the antimicrobial activity of the Tunisian Asteriscus maritimus (L.) Less essential oils obtained from flowers, leaves and stems were investigated. According to the GC and GC-MS analysis results, 45 (99.32%), 34 (94%) and 29 compounds (94.95%) were identified, respectively. In the essential oils extracted from the flowers and leaves of A. maritimus, oxygenated sesquiterpenes were abundantly found (57.82 and 46.39%, respectively). Hexdecanoic acid was detected in an important amount in leaves and stems (30.35 and 49.18%, respectively), while ?-eudesmol (24.25%), menthyl acetate (17.03%) and pentadecanal (15.38%) were the most abundant constituents in flowers. To evaluate the in vitro antimicrobial activity, all volatiles were tested against some bacterial and fungal agents. It was found that only the volatile oil from flowers exhibited interesting antibacterial and antifungal activities. When screened for their anti-acetylcholinesterase activity, essential oil from flowers exhibited the highest activity (IC50 =95 ?g/mL). To our knowledge, this is the first report of acetylcholinesterase inhibition and antimicrobial activity of the Tunisian A. maritimus essential oils.
32 An expedient approach for the synthesis and the anti-acetylcholinesterase activity evaluation of 6H-benzimidazol[1,2-c][1,3,2]benzoxazaphosphorine 2-(4-methoxyphenyl)-2-sulfide derivatives from 4-mercapto-2H-chromene-2-thione, Imen Zghab, Belsem Trimeche, Anis Romdhane, David Touboul and Hichem Ben Jannet*
A new efficient route for the synthesis of substituted 6H-benzimidazol[1,2-c][1,3,2] benzoxazaphosphorine 2-(4-methoxyphenyl)-2-sulfide from 4-mercapto-2H-chromene-2-thione is described. The anti-acetylcholinesterase activity of the most important synthons is considered. Ways of constructing six-membered phosphorus-heterocycles via cyclization of Lawessons reagent with bifunctional substrates are discussed.
33 Investigation of the Self-Diffusion Coefficients of Trivalent Gd3+ in aqueous solutions: The Effect of Hydrolysis and nitrate ion association, Rafik Besbes*, Noureddine Ouerfelli, Manef Abderabba, Patric Lindqvist-Reis and Habib Latrous
In recent work, we have deduced that berkelium and gadolinium, which have 4f and 5f with half-filled configurations, also display similar diffusion properties. Results, using self-diffusion coefficients to study thermodynamic properties, show very similar behavior, which is understood given their similarities in charge, ionic size, mobility, conductance, and hydration number. In this paper we undertook a study of Gd3+ as an aid for deducing the thermodynamics properties of the Bk3+ . In first part we compare magnitudes of transport (self-diffusion coefficient) of the trivalent aquo ions of Gd III for two concentrations, C1 = 2 10-4 mol.L-1, C2 = 10-3 mol.L-1 , and in perchlorate and nitrate media . In second part, we studied the variation of D with the mediums pH. Self-diffusion coefficients, D, of the trivalent f-elements aqua ions have been determined in an aqueous electrolyte support of Gd(NO3)3 and Nd(ClO4)3 and at a pH=2.5. (HNO3, HClO4 ) and at 25 C using the open-end capillary method (O.E.C.M.). The variation of D versus pH shows three zones We changed the NO3- counter ion with ClO4- ,and found that measurements must be carried in perchloric acid medium so as to avoid pairing phenomena. Using association constants between Gd3+ and NO3- , and a hydration constant, we estimated self-diffusion coefficients for Gd(NO3)2+ and Gd(OH)2+ . The results justified our choice of working at pH = 2.5 which constitute an optimum condition to avoid hydrolysis and pairing phenomena. Our results were confirmed by mobility measurements using an electro migration technique.
34 Synthesis and biological evaluation of new pyrazolo[3,4-d]pyrimidine derivatives, Asma Agrebi*, Fatma Allouche, Hamadi Fetoui and Fakher Chabchoub
Several new pyrazolopyrimidine compounds were achieved from aminocyanopyarazole 1. The starting material 1 was initially coupled with orthoester at refluxed with various primary amines, ammonia, hydrazines and hydroxylamine to furnish a series of pyrazolo[3,4-d]pyrimidines. The reaction of imidate 2a-b with hydrazide derivatives led to the formation of pyrazolo[3,4-d][1,2,4]triazolo[4,3-c]pyrimidines. Some of the synthesized compounds 3a and 4c were evaluated for their anti-inflammatory, antipyretic and nociceptive activities. We start by studing the toxicity of these two molecules by measuring the corresponding DL50. The DL50 of 3a and 4c are estimated to 1333.2mg / kg and 1593.5mg / kg respectively. Pharmacological evaluation showed that compounds 3a and 4c at doses (5.5-22.2 mg / Kg, i.p) exhibited anti-inflammatory activities compared to Ibuprofen (150 mg / Kg, i.p), used as a refer ence drug. Further, our study showed that the injection of derived pyrazolopyrimidines on hyperthermic animal leads to a decrease in temperature after 1 hours of treatment compared to paracetamol used as reference. In addition, the injection of derived pyrazolopyrimidines at different doses contains a potent nociceptive activity. This effect is dose-dependent compared to aspirin.
35 Differential protein expression in normal and trisomic cell lines from murine cerebral cortex measured by itraq and Mass Spectrometry, L.Leigh E. Wicki-Stordeur, Nesreen Mohammed Al Faresi, Ahmed Almehdi, Derek S. Smith, Christoph H. Borchers, Terry W. Pearson, Jody D. Haddow*
Down syndrome (DS), the most common cause of genetic mental dysfunction, is caused by aberrant protein expression due to a trisomy of chromosome 21 (Ts21). A mouse model of Ts21, based on synteny of human chromosome 21 and murine chromosome 16, is used for studying the mechanisms involved in DS. In this study we measured protein expression in immortalized cell lines derived from normal and trisomy 16 (Ts16) fetal mouse cerebral cortex (CNh and CTb respectively). iTRAQ labeling and mass spectrometry were used to examine each cell line for significant up- or down-regulation of proteins. CTb cells showed increased expression of 71 proteins and decreased expression of 56 proteins when compared to the normal CNh control cells. Several of these differentially expressed proteins have previously been reported to show aberrant expression in DS and other neurological disorders such as Alzheimers disease, a condition closely associated with Down syndrome. Our results clearly demonstrate the aberrant expression of proteins with various cellular functions within the trisomy model and may lead to a deeper understanding of the proteins and mechanisms involved in the Down syndrome phenotype.
36 Controlled Release of Benzocaine from Monomer and Copolymer Carriers in Synthetic Gastro-intestinal Media, Houaria Merine, Abderrezzak Mesli*, Nafa Chafi and Zohra Bengharez
New dosage forms able to control drug release in the gastro-intestinal media have been prepared and investigated in this paper. Two different type of medicinal agent bonding (MA), in our case Benzocaine (Bz), were chosen in order to examine drug release. i) MA attached to ethylenic monomer (m,p-vinylbenzaldehyde), condensation reaction. ii) The copolymer carrier (Cp) is obtained by copolymerizing this monomer. These two carriers were well characterized by microanalysis, FTIR, DSC (Tg) and GPC (Ip) and the two fraction ? and ? were calculated from elemental analyses of Cp. The results showed good polydispersity and low average molecular weight. MA linked to an organic product by the azomethine function (C=N), hydrolytically sensitive, allowed controlled release of Bz, from the monomer carrier and from the bending Schiff bases groups. Theoretical and experimental analyses of controlled release of Bz kinetics from monomer and copolymer carriers were conducted for the case of contact with synthetic gastro-intestinal fluids at various pH (1,2; 6,0 and 8,0) at 37C. The process was found to be controlled by the nature of media (heterogeneous), which involved the preliminary hydrolysis, and the drug (Bz) diffusing out of structure of copolymer (Cp) to the external aqueous media. The results obtained on the rate of delivery showed a clear difference between pH = 1,2 and pH = 6,0 and 8,0 based on: i) The cation of p-aminoniumbenzoic acid (PABAH+) release at pH = 1,2 ii) Bz release at pH = 6,0 and 8,0
37 Telon dye removal from Cu(II)-containing aqueous media using p-diphosphonium organo-montmorillonite , Benamar Makhoukhi, Mohamed Amine Didi*, Hidayet Moulessehoul, Abdelkrim Azzouz*
Ion-exchange of montmorillonite with para-bis(triphenyl phosphonium methylene)-benzene ions (p-TPhPMB) provided an organo-montmorillonite adsorbent with improved affinity towards Telon dyes. Adsorption tests applied to Telon-red and Telon-blue in the presence of Cu(II) cations revealed a significant increase in the maximum adsorption capacity from ca. 11-26 for the starting clay mineral to ca. 110-160 mg.g-1 after intercalation. This improvement was attributed to increases in both the organophilic character towards the organic dyestuffs investigated and the interlayers spacing. Besides dye-diphosphonium and Cu(II)-diphosphonium interactions, dye adsorption on organo-montmorillonite also involved the formation of Cu(II) exchanged Telon-dye species. It was found that dye adsorption involves not only binary interactions between the three chemical species, but also synergy due to a possible bridging action of the divalent Cu(II) cations. On organo-Mt, the organophilic character was a key factor for higher amounts of adsorbed dye.
38 Optimization of activated carbon from residues of oregano using experimental design method, Saadia Marouane*, Nazha Oumam, Abdlemjid Abourriche, Ahmed Benaamara and Mhamed Charrouf
A series of eight activated carbons were obtained by chemical activation of oregano marc, which is abundant waste in Morocco. The activated carbons responses (capacity of adsorption, and yield) were analyzed as a function of the experimental parameters (temperature, time and chemical agent), using the complete factorial design of 23 experiments. Each response has been described by a second order model that was adequate to predict responses in all experimental regions. The experimental values obtained were in good agreement with the values predicted from the models, with relatively small errors between the predicted and the actual values. The optimization of activated carbon, using the function of desirability, was carried out by JMP software. The optimal activated carbon is obtained when using 60 min as activation time, 350C as activation temperature, and H3PO4 as chemical agent.
39 Synthesis, spectroscopic and electrochemichal characterization of mixed cobalt complexes with aminoacids and isonitrosoacetophenone. Biological activities, Nabila Tidjani-Rahmouni, Safia Djebbar and Ouassini Benali-Baitich*
Complexes formed from isonitrosoacetophenone and aminoacids such as L-Phenylalanine, L-Tryptophan and L-Histidine having the formula [Co(INAP)L(H2O)2] have been synthesized. The complexes have been characterized using elemental analyses, molar conductance, UV-Vis, IR and 1H NMR spectroscopy. The value of molar conductance indicates them to be non-electrolytes. The IR spectra support the binding of the ligands with two N and two O donor sites to the cobalt(II) ion giving an arrangement of N2O2 donor group. Electrochemical behavior of the complexes have been investigated by cyclic voltammetry which shows that the chelate structure and electron donating effects of the ligand substituent are among the factors influencing the redox potentials of the complexes. The antimicrobial activities of the complexes were evaluated against several pathogenic microorganisms to assess their antimicrobial potentials. The cobalt complexes were found to be more active against Gram-positive than Gram-negative bacteria. Furthermore, the antioxidant efficiencies of the metal complexes were determined by 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical scavening activity. The antioxidant activity of the complexes indicates their high scavenging activity against the radical DPPH.
40 Synthesis, Spectroscopy and Crystal Structure of a New Copper Complex Builtup by Cationic (Dimethylphosphoryl)methanaminium Ligands, Manuela E. Richert, Cora Helmbrecht and Guido J. Reiss*
A new transition metal complex of the mono-protonated ligand (dimethylphosphoryl)methanamine (dpmaH+) was obtained by equimolar reaction of copper(II) chloride dihydrate and dpma in concentrated hydrochloric acid. The asymmetric unit of the title structure, [CuCl2(C3H11NOP)4][CuCl4]2, consists of one half of a fourfold charged trans-dichloridotetrakis[(dimethylphosphoryl)methanaminium]copper(II) complex with the copper atom located on an inversion centre and one tetrachloridocuprate(II) dianion found in a general position. The copper centre in the cationic complex shows a tetragonally distorted octahedral environment composed of four oxygen atoms in a square plane and two trans-coordinated chlorido ligands. This 4+2-coordination causes elongated Cu-Cl distances because of the Jahn-Teller effect. The geometry of the tetrachloridocuprate(II) dianion is best described as a seriously distorted tetrahedron. Analysis of the hydrogen bonding scheme by graph-set theory shows three patterns of rings in the title compound. The cationic copper complex reveals intramolecular hydrogen bonds between two aminium groups and the two axial chlorido ligands. Further hydrogen bonding among the cations and anions, more precisely between four aminium groups and the chlorido ligands of four adjacent tetrachloridocuprate(II) anions, lead to a chain-type structure. Comparing the coordination chemistry of the title structure with an analogue cobalt(II) compound only disclose differences in hydrogen bonding pattern resulting in an unusual chain propagation. Besides the crystal structure received spectroscopic data are in accordance with appropriate literature.
41 Cationic Ruthenium Complexes with an Arylspiroborate Counterion Derived from 3,5-Di-tert-butylcatechol , Jennifer A. Melanson, Graham M. Lee, Christopher M. Vogels, Andreas Decken and Stephen A. Westcott*
We have prepared ruthenium complexes containing the Bbutcat2- anion (butcat = 3,5-di-tert-butylcatecholato) and the first single crystal X-ray diffraction study of a ruthenium arylspiroborate complex is presented. These new ruthenium complexes have been examined for their ability to catalyse the addition of diorganyloxyboranes to vinylarenes, and results suggest that these compounds generate the corresponding alkenylboronate esters via a competing dehydrogenative borylation pathway.
42 Prediction of surface tension of alcohol + water solutions using artificial neural networks, Gonzalo Astray, Oscar A. Moldes, Iago A. Montoya, Juan C. Mejuto*
Different Artificial Neural Network architectures have been implemented to predict Surface Tension of aqueous solutions of methanol, ethanol, 1-propanol and 2-propanol in range temperatures of 293.15-323.15 K. Artificial Neural Networks with four entrance variables, Critical Volume, log P, Mole Fraction and Temperature, were used. Best ANN architecture was formed by four input neurons, two middle layers (with eleven and three neurons respectively) and one output neuron. Root Mean Square Errors (RMSEs) are 0.34 mNm-1 (R2= 0.9995) for the training set and 1.31 mNm-1 (R2= 0.9955) for the validation set. Those errors correspond with a 0.62% error and 4.37% of error for training and validation set, respectively. For the full data set the Root Mean Square Error is 0.72 mNm-1 (R2= 0.9976) with a 1.56% error.
43 Aspartic protease inhibitory and nematocidal activity of phenyl-4-(2-phenylhydrazono)hexahydrofuro[3,2-c]pyridazin-7-ol (Percival dianhydroosazone), El Sayed H. El Ashry*, Nighat Shamim Rizvi, Ahmed T. A. Boraei, M. Kamran Azim, Waseem Ahmed, M. Sajid and Shaikh S. Nizami
We synthesized Phenyl-4-(2-phenylhydrazono) hexahydrofuro[3,2-c]pyridazin-7-ol (compound 3). The structure compound 3 was elucidated with IR, 1H NMR, 13C NMR and EIMS spectra. Compound 3 showed potent inhibitory activity against aspartic proteases, human cathepsin D and Plasmodium falciparum plasmepsin-II with IC50 = 20 ?M. Enzyme-inhibitor complexes were predicted to stabilize by electrostatic and hydrophobic interactions between the side chains of amino acid residues at the active center and compound 3. Moreover, compound 3 displayed good nematocidal activity against all developmental stages of C. elegans.
44 Phytochemical study on the constituents from Cirsium arvense, Zia Ul Haq Khan, Farman Ali, Shafi Ullah Khan and Irshad Ali *
Phytochemical investigation on the chloroform soluble fraction of Cirsium arvense resulted in the isolation of five compounds namely Ciryneol C, Scopoletin, Pectolinarigenin-7-O-glucopyranoside, Acacetin and 6, 7-Dimethoxycoumarin. Their structures have been elucidated by EIMS, HREIMS, 1H and 13C NMR spectroscopic methods. These compounds have been isolated for the first time from this plant. All the isolated compounds were tested for their antibacterial and antifungal activities.
45 Chemical modifiers in electrothermal atomic absorption determination of Platinum and Palladium containing preparations in blood serum, ?ntonina Alemasova* and ?leg Ponomarenko
The biological liquids matrixes influence on the characteristic masses and repeatability of Pt and Pd electrothermal atomic absorption spectroscopy (ETAAS) determination was studied. The chemical modifiers dimethylglyoxime and ascorbic acid for matrix interferences elimination and ETAAS results repeatability improvement were proposed while bioliquids ETAAS analysis, and their action mechanism was discussed.
46 Quantitative proteomic analysis of differentially expressed proteins in A?(17-42) treated synaptosomes, Jaffer Mohammed, Joseph T. Johnson, Rukhsana Sultana, Joshua B. Owen, Tanea T. Reed*
Oxidative stress has been associated in the pathogenesis of numerous diseases such as various neurodegenerative disorders, ischemia, and cancer. The brain is susceptible to oxidative stress due to its high content of peroxidizable unsaturated fatty acids, high consumption of oxygen, and elevated levels of free radicals. Reactive oxygen species (ROS) and reactive nitrogen species (RNS) can react with biomolecules such as proteins, lipids, carbohydrates, DNA, and RNA, which can lead to oxidative damage, cellular dysfunction, and ultimately cell death. Down syndrome (DS) is caused by trisomy of chromosome 21, a genetic abnormality in which an extra copy of the chromosome is present. DS patients have extensive deposition of A?(17-42) peptide, which could contribute to their increased rate of developing Alzheimers disease (AD), which is consistent with current research. Since AD cannot be properly diagnosed until autopsy, development of a novel Down syndrome model using A?(17-42) could be beneficial in determining oxidative stress levels and their relationship to mild cognitive impairment (MCI), the earliest form of AD. This work will demonstrate the use of a novel Down Syndrome model and its correlation to oxidative stress. We have found a significant difference between oxidative stress levels in A?(17-42) treated synaptosomes and control. By using proteomics, we have also identified several biomarkers including aldehyde dehydrogenase, aldolase, ?-enolase, heat shock cognate 71, peptidyl-prolyl cis-trans isomerase, and ATP synthase ? chain. Our present findings suggest the role of A?(17-42) as one of the contributing factors in mediating oxidative stress in DS and AD brain leading to neurodegeneration. This novel DS model may have potential applications as a diagnostic tool to identify biomarkers that may contribute to Alzheimers disease.
47 Synthesis of two new oxaziridines and a nitrone from derivatives of aryl-substituted dihydroisoquinoline, Mouna Bouzid, Majed Kammoun*, Sihem Dhifaoui and Mohamed Damak
N-alkyl oxaziridines may be used as reagents for the oxidation of sulfides in acid-promoted reactions. This study describes the synthesis of two new oxaziridines. The reactivity of the latter was investigated in acidic medium both in presence and in absence of sulfides. In the absence of sulfides, a new nitrone was produced.
48 Evaluation of production electrocatalyst for hydrogen electrolysis from water , Miguel A. Gutirrez O., Nstor Y. Rojas, Liliana Giraldo, Juan Carlos Moreno-Pirajn*
This paper analysed three specific ternary alloys, electrodeposited on the cathode and the anode of alkaline water electrolysis, called electrocatalysts. The analysis was done by monitoring the hydrogen production (mL/min) from the electrolysis of water at different current densities (mA/cm2). Three different electrocatalysts were analysed, at the cathode (Ni, Pt and Mo) and the anode (Ni, Co and Cr). The difference between the cathode electrocatalyst was given by the composition of the nickel (54.4 wt% and 74.4 wt%), which represented a change in the structure of the phases in the electrode surface. No significant difference was found between the two different electrocatalysts at the cathode, despite the higher content of nickel and greater influence on hydrogen production. A 30% increase in the production of hydrogen with respect to the control was reached, the presence of the electrocatalyst at the anode and presence of nickel in the cathode electrocatalyst.
49 Synthesis, characterization and antibacterial activity of bis-amidrazones and bis-triazolones derivatives, Salwa Hamzaoui, Adel Ben Salem, Anis Ben Hsouna, Najla Chaari, Mohamed Trigui, Maxime Mourer and Mohamed Kossentini*
We present a new method for the synthesis of bis-triazolones 3, which result from the processing of novel bis-amidrazones 2 with ethyl chloroformate. The bis-amidrazones 2 are prepared by the reaction of the N1-tosylhydrazonates 1 with two equivalents of aliphatic diamine. The structures of the new products were determined through IR, 1H and 13C NMR studies as well as elemental analysis. The molecular structure of the compound 3c was also determined via an X-ray analysis. The antimicrobial activity of the synthesized compounds was evaluated against a panel of 09 bacterial strains using broth microdilution methods. Results showed that compounds exhibited moderate to strong antibacterial activity against the tested species.
50 Synthesis of some poly (N-2-vinyl pyrrolidone-co-metha crylamide)s as model carriers of anilines. Study of the release of anilines in aqueous heterogeneous medium of pH=1.2 at 37C., Ilham Abdelmalek, Abderrezzak Mesli*, Nacer Boudouaia, Nafa Chafi et Grard Simonneaux
Four secondary amides have been prepared by the Schotten-Baumann reaction between model anilines (Pa1-4: p-XC6H4NH2: X1: H; X2:CH3; X3:COCH3; X4: CN) and methacryloyl chloride using aqueous THF/NaOH mixture at 0C. MS1, MS2 and MS4 liquid monomers are obtained whereas MS3 is a solid monomer. Mass radical copolymerization of the different monomers (MS1-4) with N-vinyl-2-pyrrolidone yields to the corresponding four copolymers. All the monomers have been characterized by IR, 1H and 13C NMR. The (CP1-4) have been characterized by IR spectra, microanalysis, Tg and Mv. The kinetics of aniline delivery to give anilinium cations (PaH+)1-4 from solid MS3 and CP1-4 dispersed in water (pH= 1.2, 37C) showed that aniline delivery from the different supports is controlled by a diffusion process and not the rate of amide hydrolysis. The amount (%) of free anilinium cations is inversely proportional to the molecular weight of polymeric supports. Accordingly, the monomer MS3 gave the largest amount of free anilinium cations (PaH+) 1-4.
51 Incorporation of gold nanoparticles into pH responsive mixed microgel systems, Azwan Mat Lazim*, Julian Eastoe and Melanie Bradley
This research attempts to demonstrate that gold nanoparticles are stable and easily dispersed in mixed microgel systems. In order to prepare stable and controllable responsive systems, the polymers were chosen to be pH responsive. As a result, that the charge signs (+/-) and level could be readily manipulated by adjusting the background solution pH. A switchable on and off system was obtained where these composite AuMES-NP-MM systems switched from a dispersed (pH 10) to a collapsed state (pH 3). This variation in pH affected the dispersion stability due to differences in the microgel particle charges. These systems are therefore successful multifunctional systems which act as reversible scaffolds for support and entrapment of AuMES-NPs. A stability graph was plotted and based on calculation, the amount of AuNPs dispersed in the microgel were estimated. These promising results offer wide applications in various areas especially using the microgel systems as a responsive template.
52 The use of bentonite in heterogeneous medium as an efficient recyclable catalyst in the synthesis of iminoesters , Radia Kaid Slimane, Ayada Djafri*, Fatiha Djafri
A new solid catalyzed synthesis of ?-iminoesters is described. Various ?-aminoesters react readily with aryl aldehydes to produce the corresponding imines in heterogeneous medium in the presence of bentonite (montmorillonite from oust region of Algeria). The products have been isolated in good to excellent yields. This new environmentally, friendly catalyst provides significantly higher yields than traditional methods during relatively short reaction times for the preparation of the target compounds.
53 Sorption of 1Naphthol on ?CyclodextrinPoly(ethylene Glycol) hydrogels, Ivn Snchez, Luis C. Cesteros and Issa Katime*
The sorption behavior of hydrogels prepared by crosslinking ?cyclodextrin with poly(ethylene glycol) modified with isocyanate end groups, is analyzed by using 1naphthol as a model molecule. Concave sorption isotherms are observed and are well described by the Freundlich isotherm model. The sorption capacity increases as does the concentration of 1naphthol in the medium and depends on the molar mass of poly(ethylene glycol) used in the synthesis of the hydrogel and on its ?cyclodextrin content. For hydrogels with the same content of ?cyclodextrin, the sorption capacity decreases with increasing the molar mass of poly(ethylene glycol) used in the synthesis. The higher sorption capacity has been found for the hydrogels prepared from PEG with a molar mass of 400 g/mol and with a ?cyclodextrin content between 912 % in weight. The sorption capacity of these samples is close to that reported for other hydrogels based on ?cyclodextrin.
54 Synthesis and crystal structure of tetra(quinolin-8-olato)thorium ethanol solvate, Th(C9H6NO)4*C2H5OH, Holger Kohlmann
Metal quinolinolates (also known as oxinates) have been widely used for gravimetric analysis and in recent days as materials for organic light emitting diodes (OLEDs). Recrystallisation of tetra(quinolin-8-olato)thorium(IV) (ThQ4) yielded yellow, translucent, prismatic crystals of the title compound, ThQ4*C2H5OH, the single-crystal structure of which is described. Only one crystallographically distinct molecule is found, all ligands are crystallographically inequivalent. Thorium is coordinated by four 8-hydroxyquinolinato with average Th-O distances of 233.3 pm and average Th-N distances of 272.4 pm, and one ethanol ligand with a Th-O distance 256.7 pm. O and N surroundings around thorium can be described by a tricapped trigonal prism. In contrast to quinolinates of the trivalent metals, ThQ4*C2H5OH does not fluoresce under UV irradiation, which is in accordance with the lack of ?-? overlap in the crystal structure.
55 Characterization of curcumin-nicotine interaction in cetyltrimethyammonium bromide micelle, Maurice O. Iwunze
A combination of fluorescence and UV-Vis spectrophotometric techniques were used to characterize the interaction of curcumin and nicotine in a cetyltrimethylammonium bromide (CTAB) micellar system. It is observed that in this medium curcumin and nicotine interact in a 1:1 ratio using the UV-Visible molar ration method. The fluorescence spectrophotometric technique, using the Benesi-Hildebrand equation was used to determine the association constant, Ka. The value thus obtained is 1.26 0.02 x 105 M-1 and the molar absorptivity, ?, of 2.3 0.06 x 104/M-cm. The free energy of association, ?Ga, was subsequently calculated as -29.1 kJ/mol. This vale together with the value obtained for Ka implies that the complex formed by curcumin and nicotine in this medium is not only spontaneous but it also very stable.
56 The effect of ultrasound on the yields of Heck reaction using Pd-catalyst in DMF/water, Khemas Sad, Majed Kammoun, Younes Moussaoui, Ridha Ben Salem*
The heck reaction of aryl bromide with styrene in N,N-dimethyl formamide/water as solvent has been studied using different catalysts under ultrasonic irradiation at room temperature. The effect of the solvent, the base, and the catalyst of the transfer phase were studied. The results show that ultrasonic irradiation increases the heck reaction yield and becomes faster with the amount of aliquat-336.
57 Synthesis, characterization and release studies of monomer and copolymers based on 3-aminopyridine as a pharmaceutical precursor, Kheira Diaf, Zineb El bahri, Zohra Bengharez, Nafa Chafi* and Abderrazzek Mesli
The aim of the current study is to prepare controlled release formulations composed from 3-aminopyridine. This active molecule is modified by chemical grafting on monomer based on (m,p)-vinylbenzaldehyde and then copolymerized with dimethylacrylamide to get hydrosoluble systems. In these systems, the active agent is spaced out from copolymer chain by phenyl group. The obtained supports i.e. monomer and copolymers are characterized by FTIR, NMR (1H, 13C) and other techniques. The drug release from these formulations is studied and the values of release constants demonstrated that 3-aminopyridine release can be modified using these systems. Also, the effect of pH release media on the drug release is discussed.
58 The use of TiO2 as catalyst in thin film fixed bed reactor for the treatment of landfill water, Redha Kernani*, Nabil Mameri and Hakim Lounici
The main purpose of this study is the use of TiO2 as catalyst in thin film fixed bed reactor (TFBR) for the treatment of landfill water with the high initial concentration of recalcitrant organic matter. The effectiveness treatment process was determined by the evaluation of the influence of the experimental parameters such as the pH on the Chemical Oxygen Demand (COD) and NH4+ concentration. The experimental assays were performed by varying the pH value from 5 to 6. The results obtained after treatment using this process was relevant. Indeed, a decrease of about 92% of the COD was achieved at pH maintained at 5. Moreover, the value of the BOD5/COD ratio obtained indicated that the water obtained after treatment are favorable for biological treatment. However, the NH4+ concentration was not affected by this process and remained at its high value.
59 Rapid determination of nitrophenol isomers in polluted water based on multi-walled carbon nanotubes modified screen-printed electrode, Essy Kouadio Fodjo, Yuan-Ting Li, Da-Wei Li, Sara Riaz and Yi-Tao Long*
A sensitive screen-printed electrode modified with multi-walled carbon nanotubes (MWCNTs/SPE) was applied to determine simultaneously m-nitrophenol, o-nitrophenol and p-nitrophenol. The electrochemical response showed that o-nitrophenol, m-nitrophenol and p-nitrophenol were entirely separated at the MWCNTs/SPE interface. Under the optimized conditions, it was found that the detection limits were 8.110-8, 5.510-7 and 2.010-7 M and the linear calibration ranges were 1.010-6~1.910-5 M, 2.510-6~2.110-5 M and 2.010-6~2.010-5 M for m-nitrophenol, o-nitrophenol and p-nitrophenol respectively, proving that the electrode presented here could be easily used to determine nitrophenol isomers simultaneously with high sensitivity within pH range from 4.8 to 8.0. The applications in water samples showed that no interferences appeared with deviations below 5% to the determination of nitrophenol isomers with 1000 fold excess, indicating a good response of this method for nitrophenol isomers detection. This disposable modified SPE combining with a portable electrochemical device were performed for wastewater samples on-field rapid determination.
60 A review of Innovative Chemical Drawing and Spectra Prediction Computer Software, Manish Kaushik
In recent years there has been an increasing research emphasis on complex macromolecular systems. These include polymers and coordination compounds with precise control of structures, multicomponent systems with higher degrees of organization, they involved in confined environments, nanochemistry and nanostructures, biopolymers and bio-inspired chemistry. Successful Spectroscopic studies of these complexes require judicious applications of existing techniques and development of new or improved strategies and methodologies. In this article various Chemical drawing and Spectra prediction computer software are compared and analyzed for their role in research in complex macromolecular systems. We have compared various software like Accelrys (Symyx) Draw, ChemDraw (ChemBioDraw), DrawIt, ChemSketch, ChemDoodle, Chemistry 4-D Draw, MarvinSketch and MestreNova NMR Predict.
61 New polyacylhydrazone dynamers incorporating furan moieties, Ichraf Jarraya, Imen Abdelhedi, Majdi Abid, Souhir Abid* and Rachid El Gharbi
Solution polycondensation of furanic dihydrazides with different bridging groups, in conjunction with terephthaldehyde or isophthaldehyde, gave high yields of a novel series of furanic polyacylhydrazones with high molecular weights. The polymers were characterized by solubility tests, viscosity measurements, 1H and 13C NMR, FTIR spectroscopies and thermogravimetric analysis. The polyacylhydrazones obtained had inherent viscosities in the range of 0.52-1.21 dL/g, and were easily dissolved in common polar solvents. The glass-transition temperatures of these polymers were recorded between 201 and 232C. Decomposition temperature for 10% weight loss all occurred above 352C in nitrogen atmosphere.
62 Chemical Composition, Antioxidant and Anti-acetylcholinesterase activities of Tunisian Crithmum maritimum L. Essential oils, Asma Nguir, Malek Besbes, Hichem Ben Jannet*, Guido Flamini, Fthia Harzallah-Skhiri and Mhamed Ali Hamza
acetylcholinesterase properties of the aerial parts and roots essential oils from Crithmum maritimum L., Apiaceae, gathered in the area of Monastir (Tunisia). The essential oils have been analysed by GC and GC-MS. Remarkable differences were found between the constituent percentages of the different studied organs. The most important compounds from the aerial parts were: ?-terpinene (39.3%), methylcarvacrol (21.6%) and p-cymene (11.8%). In the roots oil, the main components were terpinolene (36.9%), dillapiole (26.8%) and ?-terpinene (21.9%). The antioxidant activity of the two oils was evaluated by employing 2,2-diphenyl-1-picrylhydrazyl hydrate (DPPH) and 2,2?-azino-bis(3-ethylbenzthiazoline-6-sulfonic acid) (ABTS) radical scavenging tests. The results showed that the antioxidant capacity assessed by different in vitro tests were moderate, the ABTS assay after 20 min (IC50 = 0.051 mg/mL) of aerial parts and (IC50 = 0.643 mg/mL) of the roots, appeared to be more potent than that for the DPPH assay (IC50 = 0.92 mg/mL) of aerial parts and (IC50 = 0.048 mg/mL) of roots. In addition, the examined oils showed the highest AchE inhibitory 1 mg/mL activity (31.16% and 26.35%, for the aerial parts and roots, respectively).
63 Chemical composition and antibacterial activity of Thymus zygis subsp. gracilis (Boiss.) R. Morales essential oils from Morocco, Souad Yakoubi, Ali Cherrat, Mohamed Diouri, Fatima EL Hilali and Touriya Zair*
Thymus zygis subsp. gracilis samples were collected from different Moroccan Middle Atlas sites at three phenological stages. Chemical composition of essential oils obtained from these samples was studied and their antimicrobial activity was evaluated. GC-MS analysis of essential oils shows quantitative and qualitative changes in the chemical profile. Twenty-three components were detected. These compounds fall under at least four chemical families whose relative importance varies with the sites and the phenological stages. Monoterpens were the most abundant and their percentage in essential oils varied from 61.38 to 94.91. Carvacrol (16.07 to 74.33%), thymol (1.47 to 32.46%), p-cymene (6.97 to 40.26%) and ?-terpinene (2.68 to 22%) were the main constituents. Bactericidal property of Thymus zygis essential oils was also evaluated in vitro against six strains of phytopathogenic bacteria. All bacterial strains tested were susceptible to essential oils. Maximum activity was observed against the Gram-negative bacterium Erwinia amylovora and Gram-positive actinomycete Streptomyces scabiei. The most bactericidal effect was observed against Streptomyces scabei. Its minimum bactericidal concentration (MBC) was 50 ?g.mL-1 . At post-flowering stage, carvacrol chemical profile was the most efficient.
64 Crystal structure of oxonium o-toluidinium sulfate at 100K,(C7H10N)(H3O)SO4, Chaouki Ben hassen, Mohamed Boujelbene*, Mohamed Khitouni, Joan Josep Suol and Tahar Mhiri
A simple oxonium o-toluidinium sulfate, (C7H10N)(H3O)SO4 , crystallized from water at ambient temperature was found to be monoclinic (space group P21/c) at 100K. In the crystal, the H3O+ ions and the SO42- anions are linked by O-HO hydrogen bonds, generating infinite layers lying parallel to the bc plane at x = 1/2. These layers are interconnected by the organic cations, which establish N-HO hydrogen bonds with the SO42- anions. Weak ?-? stacking interactions between the benzene rings of neighboring molecules further to stabilize the structure [centroid- centroid distance = 3.648 ].
65 Synthesis, characterization and crystal structure of new cobalt (III) complex: [Tris(1,10-phenanthroline-?2N,N) Cobalt (III)] trinitrate monohydrate [Co(C12H8N2)3](NO3)3.H2O, Jawher Abdelhak*, Saoussen Namouchi Cherni and Mohamed Faouzi Zid
We report herein the synthesis and the physicochemical characterization of a new cobalt(III) complex of formula [Co(C12H8N2)3](NO3)3.H2O. This compound has been prepared by slow evaporation at room temperature and characterized by single crystal X-ray diffraction, IR, UV-VIS spectra and thermal analysis (TG and DTA). Structural cohesion is established essentially by ?-? interactions between the rings of phenanthroline groups and intermolecular hydrogen bonds connecting the nitrate entities and uncoordinated water molecules.
66 Electrochromism and conductivity of sulfonated polyaniline films in propylene carbonate, Daiane Fossatti, Wilson Jos da Silva and Regina Maria Queiroz de Mello*
In this work we compare the spectroelectrochemical response of electrochemically deposited sulfonated polyaniline and polyaniline films. The electrochromic performance of SPAN is slightly superior to that of PANI, showing faster coloring and bleaching and slightly higher electrochromic efficiency than PANI. Furthermore, submitting SPAN to successive voltammetry scans in LiClO4/propylene carbonate constitutes a simple method to improve SPAN conductivity by a factor 20.
67 Facile and convenient new synthesis of imidazobenzimidazol-2-one and pyrimidobenzimidazol-2,3-dione derivatives , Abdelkebir Zarguil, Mohammed Saadouni, Said Boukhris*, Nouzha Habbadi, Amina Hassikou and Abdelaziz Souizi
Reaction of epoxides 1 and 2 with 2-aminobenzimidazole led to formation of imidazobenzimidazol-2-ones 4 and pyrimido[1,2-a]benzimidazol-2,3-diones 5, respectively in good yields. This same compound 5 may be obtained by another route by reacting halohydrin derivates 3 with 2-aminobenzimidazole. The mechanisms of the studied reactions are discussed.
68 NMR Investigation of the complexation of (S)-2-isopropyl-1-(o-nitrophenyl)sulfonyl)aziridine with ?-cyclodextrin, Assia Keniche , Mohamed Z. Slimani, Jos I. Miranda, Jesus M. Aizpurua, and Joseph Kajima Mulengi*
Aziridines are known to undergo hydrolysis in the presence of cyclodextrins, whereas the latter are largely investigated as potential vectors of biologically active compounds. Despite this easy cyclodextrin-induced cleavage of aziridines in aqueous medium, it was of interest to find out a model aziridine derivative that would be sufficiently water-stable and form a stable complex with ?-cyclodextrin in aqueous medium, so that it could be used as a reference in future formulations or vectorization work. Among compounds we have investigated, we found out that only (S)-2-isopropyl-1-(o-nitrophenyl)sulfonyl)aziridine complied with the above-mentioned solubility and stability requirements. NMR studies of the inclusion complex of this derivative with ?-cyclodextrin provided useful parameters related to the stoichiometry of the complex and the association constant Ka. The geometry of the complex was assessed by 2D-ROESY experiments, suggesting a deep insertion of the aziridine into the cavity of ?-cyclodextrin.
69 Comparative GC analyses of ripe fruits, leaves and floral buds essential oils of Tunisian Myrtus communis L. , Ahmed Snoussi, Faten Kachouri, Mohamed Moncef Chaabouni*, Nabiha Bouzouita
The chemical composition of essential oils obtained by hydrodistillation from Tunisian wild growing myrtle ripe fruits, leaves and floral buds was examined by GC and GC-MS. The yields of hydrodistilled oils obtained from different plant parts were: leaves 0.5%, floral buds 0.2% and ripe fruits 0.02%. Significant differences were found in the concentration of main constituents of the oils: ?-pinene [48.9% (floral buds), 34.3% (fruits), 23.7% (leaves)], 1,8-cineole [15.3% (floral buds), 26.6% (fruits), 61.0% (leaves)]. The leaves oil contained less linalool than floral buds and ripe fruits oils. Tunisian myrtle is characterized by the absence of myrtenyl acetate.
70 In vitro inhibitory effect of drinking water from south Algeria on the dissolution of dental hydroxyapatite, Hocine Bahloul, Hadja Mbarka Djellouli, Safia Taleb*, Zouaoui Rezgane, Abdelkrim Cheriti, Abderezzak Benghalem
Epidemiological surveys in Algeria conducted in the school health program show that the dental carious prevalence is about 67%. Water is the main source of fluorine, recognized as the essential chemical element to prevent carious dental For this purpose, the objective of this study is to test, in vitro, the inhibitory effect of Saharan fluoridated water for the dissolution of hydroxyapatite Ca5(PO4)3OH, under physiological conditions: acid (HNO3) at pH = 5.1 and T = 37 C. Thence, the fluoride content of drinking water of some Saharan region was measured, it varies from 0.48 to 3.87 0.05 mg / L. The Inhibitory effect of waters is between 54.28 and 83.1%, VC
71 Granulometric structure, zeta potential and differential scanning calorimetry of native starch powders from Dioscorea spp., Gildas K. Gbassi*, Christophe N. Amin, Patrick G. Atheba, Albert Trokourey, Seri Yolou and Michele Ake
Starch powders from two cultivars of Dioscorea rotundata (DR) were analysed on the physicochemical aspect. Granulometric structure, zeta potential and differential scanning calorimetry of starch powders showed the following properties. Various shapes with predominance of granule ranging from 10 to 40 ?m were noted. The zeta potential of DR went from positive values to negative values as the pH was increasing from 2 to 8. From pH 2 to 4, the zeta potential was positive. A significant difference was obtained between each value (p > 0.05). The zeta potential took a negative value from pH 5 and above. The results of thermal analysis show that starches start swelling at 68.9?1.5 ?C. Enthalpy of gelatinization was about 15 J.g-1.
72 Determination of copper in whole blood by differential pulse adsorptive stripping voltammetry, Tarik Attar, Yahia Harek and Lahcne Larabi*
A selective and sensitive method for determination of copper in blood by adsorptive differential pulse cathodic stripping voltammetry is presented. The method is based on adsorptive accumulation of the complexes of Cu (II) ions with benzenesulfonyl hydrazide onto hanging mercury drop electrode (HMDE), followed by the reduction of the adsorbed species by differential pulse cathodic stripping voltammetry. The effect of various parameters such as supporting electrolyte, concentration of benzenesulfonyl hydrazide, accumulation potential, accumulation time and stirring rate on the selectivity and sensitivity were studied. The optimum conditions for determination of copper include perchloric acid 0.03 M, concentration of benzenesulfonyl hydrazide 7.510-5 M, the accumulation potential of -350 mV (vs. Ag/AgCl), the accumulation time of 50 s, and the scan rate of 50 mV s-1. Under optimized conditions, linear calibration curves were established for the concentration of Cu (II) in the range of 0.62-275 ng mL-1, with detection limit of 0.186 ng mL-1 for Cu (II). The procedure was successfully applied to the determination of copper ion in whole blood samples.
73 Secondary metabolites and antioxidant activity of seed extracts from Solanum elaeagnifolium Cav., Houda Feki, Imed Koubaa and Mohamed Damak*
The aim of this study was to screen various solvent extracts of seeds of Solanum elaeagnifolium to display the phytochemical composition, the total phenolic content, the total flavonoid content and the antioxidant capacity in order to find possible sources for future novel antioxidants in food and pharmaceutical formulations. Various extracts of seeds of Solanum elaeagnifolium were obtained by maceration. The total phenolic content of the different extracts was determined by Folin-Ciocalteu method, and the total flavonoid content was quantified using a method based on the formation of a flavonoidaluminium complex .The antioxidant activity was essayed through some in vitro models such as the antioxidant capacity by phosphomolybdenum method, radical scavenging activity using 2,2-diphenyl-1-picryl hydrazyl (DPPH) assay and reducing power assay. The acetone extract showed the highest total phenolics (580.99 20.56 mg gallic acid equivalents/g of extract), and the highest total flavonoids (207.61 2.62 mg quercetin equivalents/g of extract). This extract showed an antioxidant activity higher than that of ?-tocopherol. These results suggest the potential of Solanum elaeagnifolium against free-radical-associated oxidative damage.
74 Synthesis and antitubercular evaluation of aryl substituted 2-oxazolines from L-amino acids, Leidiane Arajo de Souzaa, Emerson Teixeira da Silvaa , Maria Cristina Silva Lourenob and Marcus Vincius Nora de Souza*
This paper describes the synthesis and the in vitro antibacterial activity of a series of twelve substituted aryl-2-oxazolines against Mycobacterium tuberculosis. Seven compounds showed activity and two compounds exhibited a minimal inhibitory concentration (MIC) of 25 ?g/mL were not cytotoxic for the host cells in cell viability assay. These results could be a good starting point for the development of new antitubercular lead series based on this family of compounds.
75 Synthesis of novel pyrazolo[3,4-d]pyrimidinone derivatives as cytotoxic inhibitors, Ameur Rahmouni, Anis Romdhane, Malek Besbes, Nicolas Elie, David Touboul and Hichem Ben Jannet*
Various ?-fonctionalized iminoethers 2 were easily prepared from ethyl 5-amino-3-substituted-1-phenyl-1H-pyrazole-4-carboxylate 1. The reaction of iminoethers 2 with ammonia afforded 3-substitued-1-phenyl-1H-pyrazolo[3,4-d] pyrimidin-4(5H)-ones 3 which were also synthesized by the addition of formamide to ethyl 5-amino-3-substituted-1-phenyl-1H-pyrazole-4-carboxylate 1. The 5-amino-3-substitued-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-ones 4 were obtained from hydrazonolysis of iminoethers 2. Otherwise, the condensation of these intermediates 2 with a series of some primary amines and hydroxylamine led respectively, to the corresponding 3,5-disubstitued-1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-ones 5 and the 3-substitued-5-hydroxy-1-phenyl-1H-pyrazolo[3,4-d] pyrimidin-4-(5H)-ones 6. The synthesized compounds 1-6 were completely characterized by 1H NMR, 13C NMR, IR and HRMS. Some synthesized compounds were evaluated for their cytotoxic effect using the Human cervical adenocarcinoma Hela cell line.
76 Microwave dielectric properties of binary solvent water-alcohol, alcohol-alcohol mixtures at temperatures between -35C and +35C and dielectric relaxation studies, Adel Megriche*, Abdellatif Belhadj, Arbi Mgaidi
In this work, our objective was to study the complex permittivity of binary mixtures of water-ethanol, water-methanol and methanol-ethanol with various mole fractions at temperature between -35 and 35 C. Measurements were made in the frequency domain from 300 kHz to 1.3 GHz by means of an open ended coaxial line technique coupled to a network analyzer. Water-ethanol and water-methanol mixtures display a Kraszewski Law while methanol-ethanol mixture shows a Shivola-Kong Law. The static dielectric constant, ?s were obtained from the plateau of ?'(?) curve, in water rich mixture or alcohol rich mixture has similar real permittivity ?' of pure liquids. The values of ?s mixtures increase by decreasing the temperature assigned to the cooperative dynamics H-bond system in mediums. The validity of permittivity measurements according to the temperature are verified by the Queen-King Law and the constants are compared with literature data. ) 20(?? jj A The dielectric relaxation behaviour of water-ethanol mixture can be better described with a Cole-Davidson function while for methanol-ethanol one, a Debye function gives a good fit. At 25 C, the relaxation time ? in the aqueous mixtures of ethanol and methanol sharply increased with increasing alcohol concentration.
77 A facile approach towards the synthesis of functionalized indenol derivatives identified as potent anti-oxidant and anti-bacterial agents, Sonia Taktouk, Jihne Ben Kraiem, Hedia Chaabane, Jacques Lebreton and Hassen Amri*
An elegant one-pot synthesis of new indenols 2 was successfully carried out, starting from 1-hydroxy-1H-indene-2-carboxylic acid 1. Thus, esterification of acid 1 with aliphatic alcohols in toluene at reflux and a catalytic amount of para-toluenesulfonic acid afforded the corresponding alkyl esters 2 in moderate to good yields. This classical esterification process enables an efficient entry to a variety of new indenol-based molecular models 2, which could be adapted to a range of drug candidates. All the synthesized compounds 2a-e were subjected to the preliminary evaluation for their potential anti-oxidant and anti-bacterial activities. The assessment of radical scavenging capacity of the compounds 2a-e towards the stable free radical 2,2-diphenyl-1-picrylhydrazyl (DPPH) was measured and these compounds were found to scavenge DPPH free radical efficiently. Moreover, the in vitro antibacterial activity of derivatives 2a-e has been tested against a panel of pathogenic agents to show potent activity against all sensitive and resistant ones.
78 An investigation of toxic heavy metals (Pb, Cd, Cu, Cr and Zn) in Garlic (Allium sativum L.) and soil samples collected from different locations of Punjab, Pakistan using atomic absorption spectrometry, Sadia Ata, Azam Mukhtar*, Sidra Tayyab and Samina Ghafoor
The present study is based on the determination of heavy metal contents (Pb, Cd, Cu, Cr and Zn) in garlic and soil samples collected from ten different locations of Punjab, Pakistan using flame atomic absorption spectrometer. In garlic samples, Pb, Cd, Zn, Cu and Cr ranged from 4.9 to 94.6 mg/kg, 0.625 to 151.4 mg/kg, 3.7 to 56.4 mg/kg, 2.5 to 50.2mg/kg and 56.4 to 111.6 mg/kg respectively, whereas Pb, Cd, Cr, Zn and Cu in investigated soil samples ranged respectively from 57.4 to 99.6 mg/kg, 25.6 to 132.7 mg/kg, 61.7 to 115.1 mg/kg, 9.2 to 324.7 mg/kg and 15.5 to 34.5 mg/kg. Elevated concentration of Pb and Cd was found in garlic samples from Gujranwala, Cr concentration was found to be higher in samples collected from Raiwind while the other metals such as Cu and Zn were predominant in samples from Kasur. Heavy metal content in soil and garlic samples was within the permissible limits proposed by World Health Organization (WHO) except Cd, Cr and Zn which showed elevated levels in almost all soil and garlic samples. Average concentrations determined in all samples represented that metal content in soil samples was in increasing order as Zn
79 Phytochemical study and insecticidal activity of Mentha pulegium L. oils from Morocco against Sitophilus Oryzae, Nadia Zekri , Smail Amalich , Ahmed Boughdad , Mohamed Alaoui El Belghiti and Touria Zair*
There is a growing interest of industry to replace synthetic chemicals by natural products with bioactive properties from plant origin. The aim of this study was to validate the therapeutic properties of Mentha pulegium L. by conducting a phytochemical study, to determine the chemical composition of its essential oils (EO) and evaluate its insecticidal activity against stored cereals pests. Leaves and flowers of M. pulegium L. were collected from three regions of the Moroccan Middle Atlas. Phytochemical tests on pennyroyal aerial parts revealed the presence of gallic tannins, flavonoids, alkaloids, sterols and triterpenes and saponins. The chemical composition of essential oils was analyzed by gas chromatography coupled with mass spectrometry. The main components were pulegone and piperitenone. The EO from Khnifra is dominated by pulegone (81.46%), and those from Azrou and M'rirt are rich both in pulegone (68.86 and 71.97%) and piperitenone (24.79% and 26.04%) respectively. Pennyroyal oil has showed an important fumigant effect against Sitophilus oryzae (L.) adults. This effect is influenced by the tested doses and exposure periods. The potential of this plant to be used to control stored product insects was discussed.
80 Chemical preparation, kinetics of thermal behavior and infrared studies of Pb3(P3O9)2.3H2O and Cd3(P3O9)2.14H2O, Aziz Kheireddine*, Malika Tridane and Said Belaaouad*
Chemical preparation, thermal behavior, kinetic and IR studies are given for the cyclotriphosphates Pb3(P3O9)2.3H2O and Cd3(P3O9)2.14H2O. The later cyclotriphosphates have never been studied except their crystallographic characterization and are stable in the conditions of temperature and pressure of our laboratory until 343K. The final products of the dehydration and calcination of Pb3(P3O9)2.3H2O and Cd3(P3O9)2.14H2O, under atmospheric pressure, are respectively their long chain polyphosphates, [Pb(PO3)2]? and ?[Cd(PO3)2]?. The intermediate product of the dehydration of Cd3(P3O9)2.14H2O, under atmospheric pressure, is its long chain polyphosphate form ?, ?[Cd(PO3)2]?. [Pb(PO3)2]? and ?[Cd(PO3)2]? are stable until their melting points at respectively 946K and 1153K. Two different methods, Ozawa and KAS have been selected in order to study the kinetics of thermal behavior of the cyclotriphosphates Pb3(P3O9)2.3H2O and Cd3(P3O9)2.14H2O for the first time. The kinetic and thermodynamic features of the dehydration, of the cited cyclotriphosphates, were determined and discussed on the basis of their crystalline structure. [Pb(PO3)2]?, ?[Cd(PO3)2]? and ?[Cd(PO3)2]? have many applications in industry such as corrosion inhibitors.
81 Catalytic oxidation of methanol on Pt/X (X = CaTP, NaTP) electrodes in sulfuric acid solution, Naima Farfour, Mohamed El Mahi Chbihi, Driss Takky, Khadija Eddahaoui and Said Benmokhtar*
In this paper, we report the synthesis and characterization of electrodes based on NASICON type phosphates. The study of the electrochemical oxidation of methanol at ambient temperature on electrodes based on NASICON type Ca0,5Ti2(PO4)3 (CaTP) and Na5Ti(PO4)3 (NaTP) compared to that of the platinum electrode model has been conducted by cyclic voltammetry in acidic medium. The results showed a significant increase of current density on the electro oxidation of methanol on the material developed based NASICON structure CaTP, cons deactivation of the electro oxidation is observed the closed structure type NaTP.
82 Physico-Chemical Characterization and Interfacial Electrochemical Properties of Nanoparticles of Anatase-TiO2 Prepared by the Sol-Gel Method, Ikram Daou, Rachid Chfaira, Omar Zegaoui*, Zakaria Aouni and Hammou Ahlafi
In this work, we prepared by the sol-gel method titanium dioxide nanoparticles having a large specific area (SBET = 218 m2/g). The isotherm of N2 adsorption-desorption at 77K revealed that it concerns a mesoporous solid with a maximum pore diameter of 43 . The X-ray diffraction showed that the solid is constituted of the anatase phase. The transmission electron microscopy revealed us that the synthesized grains of TiO2 are of nanometric sizes (diameter between 8 and 20 nm) and manifest under agglomerated shape. The study of its solubility in dispersing phase, by conductometric titrations, showed that the prepared solid is totally insoluble in all the domain of the studied pH. The measured inter-facial electrochemical properties, based on the isotherms of ionic adsorption and the conductometric titrations, are: the point of zero charge found equal to 6,20,1, the total number of sites of surface found equal to 5,8 OH/nm2 and the nature of action of the dispersed phase on the dispersing phase which is found organizer of the structure of water. Besides, the difference of the ionization constants ?pK is found superior to 4 for all the adsorbed ions and the constants of surface complexation are independent from the nature of the adsorbed ion.
83 Hydrothermal synthesis and crystal Structure of a new coordination polymer: [Zn1(deta)(btec)(H2O)2]n, Manel Halouani*, Mohamed Abdelhedi, Mohamed Dammak, Nathalie Audebrand and Lilia Ktari
A new metalorganic compound [Zn1(deta)(btec)(H2O)2]n where (deta= Diethylenetriamine) and (btec= benzenetetracarboxylic acid) (I) was hydrothermally synthesized from an aqueous solution of Zn(NO3)2 6H2O, (deta) and (btec). Compound I crystallizes in the monoclinic system with the P21/c space group. The unit cell parameters are a= 9.6716(5), b= 14.3776(8), c= 13.5306(8), ?= 105.311(3), Z= 4, V= 1814.71(18) 3 and Dx= 1.657 g/cm3. The refinement converged into R= 0.045, Rw= 0.048. The structure, determined by single crystal X-ray diffraction, consists of a network of ZnO4 centers, tetrahedrally coordinated by pyromellitate anions giving rise to a two-dimensional sheet structure. The connectivity resembles a 4-connected network in which each Zn atom is connected to four btec anions and each btec anion is linked to four Zn2+ ions.
84 1,3-Dipolar cycloaddition of azomethine ylide from Phtaloylimidophenylalanyl-2-hydroxymethylaziridine, Assia Keniche, Wassila Drici, Mohamed Zakaria Slimani, Abdelmoumen Mezrai and Joseph Kajima Mulengi*
Phtaloylimidophenylalanyl-2-hydroxymethylaziridine has been used as a starting material to yield azomethine ylide through thermal opening and was then involved into 1,3-dipolar cycloaddition reactions. Different five-membered adducts were obtained and were fully identified. The latter might be considered useful starting materials for further functionalization to provide novel compounds of biological interest.
85 Evaluation of antimicrobial and antioxidant activities of solvent extracts of Anacyclus pyrethrum L., from Algeria, Chaouki Selles, Mohammed El Amine Dib*, Hocine Allali and Boufeldja Tabti
In the present study, solvent extracts from aerial parts of Anacyclus pyrethrum L. were assessed for their total phenol content, antimicrobial and antioxidant (1,1-diphenyl-2-picrylhydrazyl free radical scavenging and ferric-ion reducing power) activities. The amounts of total phenolics and flavonoids in the solvent extracts were determined spectrometrically. (310.78 mg GA/g extract) and antioxidant activity (IC50 = 0.056 mg/mL). Increasing the concentration of the extracts resulted in increased ferric reducing antioxidant power for both extracts tested. The methanolic extract exhibited the best antimicrobial activity against three gram-positive bacterium (Listeria monocytogenes: 100%, Bacillus. cereus: 69% and Staphylococcus aureus: 66%), as well as against Candida albicans (81%). Finally, a relationship was observed between the biological activities potential and total phenolic and flavonoid levels of the extract. The results of this study provided an alternative of utilising Anacyclus pyrethrum aerial parts as readily accessible source of natural antioxidant in food cosmetic and pharmaceutical industry. In the present study, solvent extracts from aerial parts of Anacyclus pyrethrum L. were assessed for their total phenol content, antimicrobial and antioxidant (1,1-diphenyl-2-picrylhydrazyl free radical scavenging and ferric-ion reducing power) activities. The amounts of total phenolics and flavonoids in the solvent extracts were determined spectrometrically. (310.78 mg GA/g extract) and antioxidant activity (IC50 = 0.056 mg/mL). Increasing the concentration of the extracts resulted in increased ferric reducing antioxidant power for both extracts tested. The methanolic extract exhibited the best antimicrobial activity against three gram-positive bacterium (Listeria monocytogenes: 100%, Bacillus. cereus: 69% and Staphylococcus aureus: 66%), as well as against Candida albicans (81%). Finally, a relationship was observed between the biological activities potential and total phenolic and flavonoid levels of the extract. The results of this study provided an alternative of utilising Anacyclus pyrethrum aerial parts as readily accessible source of natural antioxidant in food cosmetic and pharmaceutical industry.
86 Cementing Material From Rice Husk-Broken Bricks-Spent Bleaching Earth-Dried Calcium Carbide Residue, Muthengia Jackson Washira*, Muthakia Gerald Kanyago and Thiongo Joseph Karanja
A cementious material, coded CSBR (Carbide residue Spent bleaching earth Broken bricks and Rice husks), was made from dried calcium carbide residue (DCCR) and an incinerated mix of rice husks (RH), broken bricks (BB) and spent bleaching earth (SBE). Another material, coded SBR (Spent bleaching earth Broken bricks and Rice husk ash), was made from mixing separately incinerated RH, SBE and ground BB in the same ash ratio as in CSBR. When CSBR was inter-ground with Ordinary Portland Cement (OPC), it showed a continued decrease in Ca(OH)2 in the hydrating cement as a function of curing time and replacement levels of the cement. Up to 45 % replacement of the OPC by CSBR produced a Portland pozzolana cement (PPC) material that passed the relevant Kenyan Standard. Incorporation of the CSBR in OPC reduces the resultant calcium hydroxide from hydrating Portland cement. The use of the waste materials in production of cementitious material would rid the environment of wastes and lead to production of low cost cementitious material.
87 Synthesis of bicyclic oxepanes: an enantioselective approach to the western part of Shaagrockol C, Boudjema Menhour*, Paul Aclinou and Jean-Pierre Pete
In this paper, we wish to report an efficient and flexible synthetic strategy towards the synthesis of Shaagrockol C. The strategy involves the construction of a bicyclic oxepane which possess several chiral centres. Such system is present in some complex natural products.
88 Fluorescence quenching of uric acid solubilized in bicontinuous microemulsion by nitrobenzene, Maurice O. Iwunze
Uric Acid is known to be practically insoluble in aqueous and alcoholic media. However, it exhibits a reasonable solubility in a Bicontinuous Microemulsion system a 15-fold or more increase in solubility in this system compared to its solubility in water. The bicontinuous microemulsion is made up of three components Dodecane-Surfactant-water. Uric acid solubilized in this system is quenched by nitrobenzene. The obtained fluorescence data do not obey the Stern-Volmer equation when plotted accordingly. Therefore, the modified Stern-Volmer equation was used to analyze the data. It was observed that only one third (1/3) of uric acid is accessible to quenching in this medium and the reaction is diffusion-limited. The Stern-Volmer quenching constant, KSV, was calculated to be 130 M-1 and the fluorescence lifetime, ?0, the quantum yield,?, and the bimolecular quenching rate constant, kq, were calculated as 10.6 nanoseconds, 0.06 and 1.23?1010 M-1s-1, respectively.
89 Kinetics of N-Deacetylation of Chitin Extracted from Shrimp Shells Collected from Coastal Area of Morocco, Hammou Ahlafi*, Hamou Moussout, Fatima Boukhlifi, Mostafa Echetna, Mohamed Naciri Bennani and Slimani My Slimane
Chitosan was obtained from the alkaline N-deacetylation of ?-chitin, derived from shrimp shells (SS) collected from the Moroccan coast. Effects of temperature, NaOH concentration and reaction time on the kinetics of deacetylation were studied. The degree of deacetylation (DD = 75%) was obtained at T = 120 C and CNaOH = 12N in a single step for 6h. It was found, from FTIR studies, that the removal of acetyl groups from chitin occur very fast for the reaction time t < 180 min and then becomes constant after, revealing two steps in the deacetylation of chitin following a first-order kinetics for each of them. The second step is considered the limiting step that has, in the temperature range of 25 120 C and maintained CNaOH = 12N, a low apparent rate constant. The activation energy of this step is about 48.76 kJ/mol. The biopolymer (Chitin and chitosan) produced were characterized by X-ray diffraction.
90 Synthesis, Cytotoxicity and Antileishmanial Activity of Aza-stilbene derivatives, Daniela T. S. de Paula, Gustavo S. G. de Carvalho, Ayla C. Almeida1, Mariana Loureno, Adilson D. da Silva, Elaine S. Coimbra*
Stilbenes are compounds found in numerous medicinal plants and food products with some known biological and even antileishmanial activity. This paper describes the preparation of Aza-stilbene derivatives and their in vitro biological activities against Leishmania species. Most of the compounds with hydroxyl groups (2a, 2b, 2d, 2e and 2f) showed interesting results against three Leishmania species tested. Compound 2f showed the best activity against intracellular forms of L. amazonensis, with IC50 of 7.48 ?M, very similar when compared to reference drug Miltefosine. It not possible associate NO production with leishmanicidal activity for all aza-stilbene derivatives. It is noteworthy that none of compounds tested showed cytotoxicity against macrophages.
91 Preparation and Characterization of NaA Zeolite Membranes and its Application for Removal of Heavy Metals , Najib Tijani, Hammou Ahlafi *, Monique Smaihi and Abdeslam El Mansouri
In this work, the characteristics of low cost NaA zeolite membranes for heavy metal removal from synthesised solutions are presented. These membranes were elaborated on a clay macroporous support which were prepared and characterized by XRD, SEM and N2 permeation. The effects of synthesis parameters such as temperature T and time t on the proprieties of the NaA zeolite membranes were investigated. The best experimental conditions for synthezised membranes are obtained for T = 60 C, t = 24 h and 117 L m-2 h-1 bar-1 for a water flux of membrane. The tests for the removal of Pb(II), Zn(II) and Cr(VI), conducted on these NaA zeolite membranes, show respectively the rejection reached 99%, 99% and 12% after 1 hour of filtration at 7 bars of N2 and at ambient temperature.
92 Evaluation of the interaction potential of synthetic ethylene glycol compounds with nuclear Factor ?B, Srinivasan Narasimhan*, Amin F. Majdalawieh, Imad A. Abu-Yousef*, Dhivya Shanmugarajan, Vishvanathan Ramasubramanian
In the last three decades, nuclear factor ?B (NF-?B) has been the focus of many researchers who are interested in understanding the various molecular mechanisms involved in inflammatory diseases and cancer. Interference with NF-?B activity can cause many cellular abnormalities including tumorigenesis. In this study, we focus on examining the potential of ten synthetic ethylene glycol based compounds to interact with the binding site of NF-?B. Computational analysis reveals that the ethylene glycol compounds examined in this study display differential ability to interact with NF-?B. Parameters such as ALOGP, dock score, and internal energy were determined for each of the studied compounds. Seven compounds were found to interact with specific amino acid residues within the binding site of NF-?B. The specific amino acids involved in the interaction were mapped and the nature of interaction was identified. Since NF-?B is implicated in the development of many inflammatory and immune-related conditions including cancer, we predict that the ethylene glycol compounds examined in this study can be targeted for the development of therapeutic agents that can be employed in the prevention and/or treatment of various diseases including cancer.
93 1,3-Dipolar cycloaddition of azomethine ylide from Phtaloylimidophenylalanyl-2-hydroxymethylaziridine, Assia Keniche, Wassila Drici, Mohamed Zakaria Slimani, Abdelmoumen Mezrai and Joseph Kajima Mulengi*
Phtaloylimidophenylalanyl-2-hydroxymethylaziridine has been used as a starting material to yield azomethine ylide through thermal opening and was then involved into 1,3-dipolar cycloaddition reactions. Different five-membered adducts were obtained and were fully identified. The latter might be considered useful starting materials for further functionalization to provide novel compounds of biological interest.
94 Use of kitchen steel wool as oxygen absorber improves storage retention of beta-carotene in solar-dried vegetables, Hudson Nyambaka*, James Nderitu, Mildred Nawiri and Jane Murungi
Vitamin A deficiency remains a major health concern in developing countries whereas the season availability of vegetables could provide for vitamin A. Dehydration is widely used to preserve dark green leafy vegetables (DGLV) but storage in normal atmosphere condition losses beta-carotene by oxidation, therefore requiring use of an oxygen absorber. The study examined use of kitchen steel wool as an oxygen absorber in reducing the loss of beta-carotene content in three indigenous DGLVs that were solar dried and stored for a period of 168 days in four different packing conditions. Fresh vegetables contained between 781.94 to 1047.42 ?g/g dry matter (DM) beta-carotene, reducing significantly (p=0.01) to between 653.63 to 712.99 ?g/g DM after dehydration. Steel wool oxygen absorber significantly improved (p = 0.02) beta-carotene retention, recording a loss of 19.5 to 37.6% compared to 47 to 72% in normal conditions. Storage of DGLVs under kitchen steel wool oxygen absorber preserves vegetables and retains high levels of beta-carotene.
95 Investigation of the Self-Diffusion Coefficients of Trivalent Gd3+ in aqueous solutions: The Effect of Hydrolysis and nitrate ion association, Rafik Besbes * 2,3, Noureddine Ouerfelli 1, Manef Abderabba 3, Patric Lindqvist-Reis 4 and Habib Latrous 1
In recent work, we have deduced that berkelium and gadolinium, which have 4f and 5f with half-filled configurations, also display similar diffusion properties. Results, using self-diffusion coefficients to study thermodynamic properties, show very similar behavior, which is understood given their similarities in charge, ionic size, mobility, conductance, and hydration number. In this paper we undertook a study of Gd3+ as an aid for deducing the thermodynamics properties of the Bk3+ . In first part we compare magnitudes of transport (self-diffusion coefficient) of the trivalent aquo ions of Gd III for two concentrations, C1 = 2 10-4 mol.L-1, C2 = 10-3 mol.L-1 , and in perchlorate and nitrate media . In second part, we studied the variation of D with the mediums pH. Self-diffusion coefficients, D, of the trivalent f-elements aqua ions have been determined in an aqueous electrolyte support of Gd(NO3)3 and Nd(ClO4)3 and at a pH=2.5. (HNO3, HClO4 ) and at 25 C using the open-end capillary method (O.E.C.M.). The variation of D versus pH shows three zones We changed the NO3- counter ion with ClO4- ,and found that measurements must be carried in perchloric acid medium so as to avoid pairing phenomena. Using association constants between Gd3+ and NO3- , and a hydration constant, we estimated self-diffusion coefficients for Gd(NO3)2+ and Gd(OH)2+ . The results justified our choice of working at pH = 2.5 which constitute an optimum condition to avoid hydrolysis and pairing phenomena. Our results were confirmed by mobility measurements using an electro migration technique.
96 Analysis of chemical composition of high viscous oils , Irina Germanovna Yashchenko and Yury Mikhailovich Polishchuk *
The spatial distribution of viscous oils which are considered as an important reserve for oil-production in future were studied on base of information from global database on oil physical and chemical properties. Changes in chemical composition of viscous oils in different basins and continents were analyzed as well. It is shown, on average, viscous oils are sulfur-bearing, low paraffin, highly resinous oils with an average content of asphaltenes and low content of the fraction boiling at 200 ?C. Study results of viscous oils peculiarities of Canada, Russia and Venezuela are given. The analysis results can be used to determine the optimal layouts and conditions of oil transportation, to improve the search methods of geochemical exploration, and to solve other problems in the oil chemistry.
97 Characterization of curcumin-nicotine interaction in cetyltrimethyammonium bromide micelle, Maurice O. Iwunze
A combination of fluorescence and UV-Vis spectrophotometric techniques were used to characterize the interaction of curcumin and nicotine in a cetyltrimethylammonium bromide (CTAB) micellar system. It is observed that in this medium curcumin and nicotine interact in a 1:1 ratio using the UV-Visible molar ration method. The fluorescence spectrophotometric technique, using the Benesi-Hildebrand equation was used to determine the association constant, Ka. The value thus obtained is 1.26 0.02 x 105 M-1 and the molar absorptivity, ?, of 2.3 0.06 x 104/M-cm. The free energy of association, ?Ga, was subsequently calculated as -29.1 kJ/mol. This vale together with the value obtained for Ka implies that the complex formed by curcumin and nicotine in this medium is not only spontaneous but it also very stable.
98 Synthesis, characterization and crystal structure of new cobalt (III) complex: [Tris(1,10-phenanthroline-?2N,N) Cobalt (III)] trinitrate monohydrate [Co(C12H8N2)3](NO3)3.H2O, Jawher Abdelhak*, Saoussen Namouchi Cherni and Mohamed Faouzi Zid
We report herein the synthesis and the physicochemical characterization of a new cobalt(III) complex of formula [Co(C12H8N2)3](NO3)3.H2O. This compound has been prepared by slow evaporation at room temperature and characterized by single crystal X-ray diffraction, IR, UV-VIS spectra and thermal analysis (TG and DTA). Structural cohesion is established essentially by ?-? interactions between the rings of phenanthroline groups and intermolecular hydrogen bonds connecting the nitrate entities and uncoordinated water molecules.
99 Synthesis and biological evaluation of new pyrazolo[3,4-d]pyrimidine derivatives, Asma Agrebi1,*, Fatma Allouche1, Hamadi Fetoui2 and Fakher Chabchoub1
Several new pyrazolopyrimidine compounds were achieved from aminocyanopyarazole 1. The starting material 1 was initially coupled with orthoester at refluxed with various primary amines, ammonia, hydrazines and hydroxylamine to furnish a series of pyrazolo[3,4-d]pyrimidines. The reaction of imidate 2a-b with hydrazide derivatives led to the formation of pyrazolo[3,4-d][1,2,4]triazolo[4,3-c]pyrimidines. Some of the synthesized compounds 3a and 4c were evaluated for their anti-inflammatory, antipyretic and nociceptive activities. We start by studing the toxicity of these two molecules by measuring the corresponding DL50. The DL50 of 3a and 4c are estimated to 1333.2mg / kg and 1593.5mg / kg respectively. Pharmacological evaluation showed that compounds 3a and 4c at doses (5.5-22.2 mg / Kg, i.p) exhibited anti-inflammatory activities compared to Ibuprofen (150 mg / Kg, i.p), used as a refer ence drug. Further, our study showed that the injection of derived pyrazolopyrimidines on hyperthermic animal leads to a decrease in temperature after 1 hours of treatment compared to paracetamol used as reference. In addition, the injection of derived pyrazolopyrimidines at different doses contains a potent nociceptive activity. This effect is dose-dependent compared to aspirin.
100 Mutagenic and genotoxic effects of wastewater detected by the Allium test, Mokhtar Chaik 1,*, Sana El Fadeli 1, Azeddine Sedki 1 and Nadra Lekouch 2,*
Screening for mutagens in complex environmental mixtures, such as industrial wastewater, is gradually being accepted as a routine method in environmental monitoring programs. The present study was carried out to evaluate the potential toxic and genotoxic effects of Marrakeshs CMR wastewater, collected from Draa Lasfar mine located about 12km south-West of the city of Marrakech, Morocco. The results from the Allium test indicate that wastewater at 100 % concentration inhibits root growth and mitotic indices; induces binucleated cells as a function of the proportion, but is not toxic at very low concentrations. Marrakesh's wastewater CMR leads to a decontrol in the cellular division, bringing about polyploid cells. In this work, we show the evidences that the exceeding genetical material of theses polyploidizated cells tend to be eliminated from the nucleus in the form of micronucleus. Our analyses prove this fact, both by the presence of a number of cells carrying a micronucleus, and by the evidences of the elimination of the exceeding material itself. The wastewater sample was analyzed by flame atomic absorption spectrometer for Zn, Pb, Cu and Cd, whose presence could partly be responsible for the toxicity of wastewater. The study concludes that the classical Allium test can give a more comprehensive data when done in combination with analysis by flame atomic absorption spectrometer. Also when wastewater is used for other purposes in combination with soils, it should be judiciously used at very low concentrations in order to protect the ecosystem health from any potential adverse effects.
101 In vitro inhibitory effect of drinking water from south Algeria on the dissolution of dental hydroxyapatite , Hocine Bahloul 1, Hadja Mbarka Djellouli 1, Safia Taleb 1,*, Zouaoui Rezgane 1 Abdelkrim Cheriti 2, Abderezzak Benghalem 1
Epidemiological surveys in Algeria conducted in the school health program show that the dental carious prevalence is about 67%. Water is the main source of fluorine, recognized as the essential chemical element to prevent carious dental For this purpose, the objective of this study is to test, in vitro, the inhibitory effect of Saharan fluoridated water for the dissolution of hydroxyapatite Ca5(PO4)3OH, under physiological conditions: acid (HNO3) at pH = 5.1 and T = 37 C. Thence, the fluoride content of drinking water of some Saharan region was measured, it varies from 0.48 to 3.87 0.05 mg / L. The Inhibitory effect of waters is between 54.28 and 83.1%, VC
102 Microwave dielectric properties of binary solvent water-alcohol, alcohol-alcohol mixtures at temperatures between -35C and +35C and dielectric relaxation studies, Adel Megriche1*, Abdellatif Belhadj2, Arbi Mgaidi1
In this work, our objective was to study the complex permittivity of binary mixtures of water-ethanol, water-methanol and methanol-ethanol with various mole fractions at temperature between -35 and 35 C. Measurements were made in the frequency domain from 300 kHz to 1.3 GHz by means of an open ended coaxial line technique coupled to a network analyzer. Water-ethanol and water-methanol mixtures display a Kraszewski Law while methanol-ethanol mixture shows a Shivola-Kong Law. The static dielectric constant, ?s were obtained from the plateau of ?'(?) curve, in water rich mixture or alcohol rich mixture has similar real permittivity ?' of pure liquids. The values of ?s mixtures increase by decreasing the temperature assigned to the cooperative dynamics H-bond system in mediums. The validity of permittivity measurements according to the temperature are verified by the Queen-King Law and the constants are compared with literature data. The dielectric relaxation behaviour of water-ethanol mixture can be better described with a Cole-Davidson function while for methanol-ethanol one, a Debye function gives a good fit. At 25 C, the relaxation time ? in the aqueous mixtures of ethanol and methanol sharply increased with increasing alcohol concentration.
103 Comparative GC analyses of ripe fruits, leaves and floral buds essential oils of Tunisian Myrtus communis L., Ahmed Snoussi, Faten Kachouri, Mohamed Moncef Chaabouni*, Nabiha Bouzouita1,
The chemical composition of essential oils obtained by hydrodistillation from Tunisian wild growing myrtle ripe fruits, leaves and floral buds was examined by GC and GC-MS. The yields of hydrodistilled oils obtained from different plant parts were: leaves 0.5%, floral buds 0.2% and ripe fruits 0.02%. Significant differences were found in the concentration of main constituents of the oils: ?-pinene [48.9% (floral buds), 34.3% (fruits), 23.7% (leaves)], 1,8-cineole [15.3% (floral buds), 26.6% (fruits), 61.0% (leaves)]. The leaves oil contained less linalool than floral buds and ripe fruits oils. Tunisian myrtle is characterized by the absence of myrtenyl acetate.
104 Fluorescence study, Raman spectroscopy, crystal structure, antimicrobial and antioxidant activities of cobalt (III) complex with a tridentate coumarin ligand, Imen Ketata, Taroub Bouzaiene, Tacir Ben Ayed1, and Rached Ben Hassen*
: Cobalt (III) complex diamine chloride was obtained from the reaction of Co (OAc)2, 4H2O; ethylene diamine and 3-acetyl-4-hydroxy-chromene- 2-one. The obtained product was characterized by Raman scattering, fluorescence and UV-visible spectroscopy. The room temperature structure was determined by single-crystal X-ray diffraction. The purity of the product was checked by X-ray powder diffraction analysis. Rietveld refinement using powder XRD confirms structure model determined by single-crystal X-ray diffraction (space group Pcca, a = 20.599(2) , b = 7.888(4) , c = 18.3820(1) and Z = 4). The metal complex was checked for its antimicrobial activity using well diffusion method and shows significant results by comparison with commercial antibiotics. Antioxidant tests indicate that the complex is an effective DPPH radical scavenger with an IC50 value of 26.32 M.
105 Determination of copper in whole blood by differential pulse adsorptive stripping voltammetry, Tarik Attar, Yahia Harek and Lahcne Larabi *
A selective and sensitive method for determination of copper in blood by adsorptive differential pulse cathodic stripping voltammetry is presented. The method is based on adsorptive accumulation of the complexes of Cu (II) ions with benzenesulfonyl hydrazide onto hanging mercury drop electrode (HMDE), followed by the reduction of the adsorbed species by differential pulse cathodic stripping voltammetry. The effect of various parameters such as supporting electrolyte, concentration of benzenesulfonyl hydrazide, accumulation potential, accumulation time and stirring rate on the selectivity and sensitivity were studied. The optimum conditions for determination of copper include perchloric acid 0.03 M, concentration of benzenesulfonyl hydrazide 7.510-5 M, the accumulation potential of -350 mV (vs. Ag/AgCl), the accumulation time of 50 s, and the scan rate of 50 mV s-1. Under optimized conditions, linear calibration curves were established for the concentration of Cu (II) in the range of 0.62-275 ng mL-1, with detection limit of 0.186 ng mL-1 for Cu (II). The procedure was successfully applied to the determination of copper ion in whole blood samples.
106 Alternative method to predict activity coefficients at infinite dilution of hydrocarbons in aqueous solutions, Gonzalo Astray*, Jorge Morales, Miriam Gonzlez-Temes, Juan C. Mejuto1, Augusto J. Magdalena
Activity coefficients at infinite dilution are important property in solute-solvent interactions. Experimental techniques show high costs, skilled labour and safety. To solve this, a neural network model with five different topological descriptors to implement different Artificial Neural Network has been implemented. The best Artificial Neural Network (5-11-8-1 topology) presents good fits for the training phase with an Average Percentage Deviation of 1.85%. Similar results have been obtained for the validation phase of the Artificial Neural Network (1.88%). The implemented Neural Networks techniques showed better results than other developed methods, around 30.70% and 24.60% for training and validation phase, respectively.
107 Coumarin derivatives: Synthesis and cation binding properties, Olfa Naouali, Rached Frija, Wissal Elgabsi, Naceur Hamdi* and Lassaad Baklouti
Coumarin derivatives were easily prepared starting from 7-hydroxy 4-methyl-2H-chromen-2-one with 40% formaldehyde and suitable secondary amines in 95% ethanol in rather good yield. The structures of all compounds were confirmed via spectroscopic techniques IR, 1H NMR, 13C NMR, mass spectra and elemental analysis. The complexing properties of the coumarin derivatives toward alkali metal, alkaline earth metal, some transition metals and some heavy metal cations have been investigated in methanol by means of UV spectrophotometry absorption and conductivity methods. Thus, the stoichiometry of the complexes formed and their stability constants were determined
108 Laser irradiation effects on ultrafine carbon-coated LiFePO4 using a modified solid state synthesis and olive oil as carbon source, Ghazi Ben Amor*, Noureddine Amdouni, Habib Boughzala and Jean Marc Grenche
Nano-size LiFePO4/C composite was synthesized via a modified solid state reaction method. Olive oil is used as carbon source. The conventional solid state process was modified by introducing two initial steps of slurry phase blending of the ingredients and solvent removal by rotary evaporation, so as to get an intimate mixing and homogenous dispersion of reactants and conductive carbon in the sample. Both structure and morphology of the LiFePO4/C composite sample have been characterized by X-ray diffraction (XRD), Mssbauer spectrometry, transmission electron microscopy (TEM) and Raman spectroscopy. The LiFePO4/C composite exhibited a high crystallinity. The particles of synthesized LiFePO4/C were fine and homogeneous in size, with an average diameter of 100nm. Since the thermal effect of laser irradiation may possibly alter material surface, particular attention has been paid in characterizing the structure and component of the material surface by Raman spectroscopy. Electrochemical measurements show that the LiFePO4/C composite cathode delivers an initial discharge capacity of 146 mAh g?1 between 2.5 and 4.3Vat a C/10 rate (a charger rated C/10 would return the battery capacity in 10 hours).
109 Utilization of waste Tunisian palm tree date as low-cost adsorbent for the removal of dyes from textile wastewater, Sami Guiza*, Khadija Ghiloufi and Final Mohamed Bagane
The removal of dyes such, as methylene blue and Congo red, from an aqueous solution is studied by adsorption Tunisian palm tree date. The equilibrium isotherm for each dye-adsorbent system was determined. The experimental results have been fitted with Langmuir and Freundlich isotherms. The maximum adsorption capacities of palm tree date are found to be 200 and 90 mg/g at dyes of methylene blue and Congo red, respectively. A comparative cost study, based on the adsorption capacity alone, has shown that the costs of the required adsorbent are 1.1%, and 1, 8%, respectively, compared with the case of commercial granular activated carbon. The Gibbs free energy values obtained confirm that the process is feasible and spontaneous G < 0. The negative values of H indicate that an exothermic chemisorption took place. The negative values of S suggest that the randomness decreases after adsorption.
110 Chemical composition, antibacterial and antifungal activities of the Cedrus atlantica (Endl.) Manettiex Carrire seeds essential oil, Rachid Rhafouri, Badr Strani, Touria Zair, Mohamed Ghanmi, Abderrahman Aafi, Mohamed El Omari and Amar Bentayeb
The Atlas cedar is an endemic species of the African North Mountains. The goal for which this work was conducted is to determine the chemical composition and to study the antibacterial and the antifungal activity of the hydrodistilized essential oil from both the winged and wingless seeds of the High Atlas Cedrus atlantica (Morocco). The essential oil is analyzed by gas chromatography and gas chromatography mass spectrometry. The essential oil yields of winged as well as wingless seeds were respectively 2.6% and 3.6%.The main constituents of the cedar wingless seeds are the ?-pinene, the manool, and the bornyl acetate; whereas, the major constituents of the cedar winged seeds are the manool and the ?-pinene. The antibacterial and antifungal activities of the essential oils were tested on four bacteria, three molds and four fungi of wood rot. The fungal strains tested were revealed more sensitive to the essential oil studied than the bacterial strains
111 Effect of thyme and myrtle leaves essential oils on the quality characteristics of cured sausage during storage, Hayet Ben Haj Koubaier, Ahmed Snoussi, Ismahen Essaidi, Soumaya Hchaichi and Nabiha Bouzouita
The aim of this work was to study the effect of adding thyme and myrtle essential oils (TEO and MEO) at different concentrations (0.05 and 1%) on the microbiological and sensorial characteristics of cured sausage during storage (21 days) at +4C. The chemical composition of essential oils, obtained by hydrodistillation, was analyzed using GC and GC-MS. Twenty and twenty three compounds were identified for thyme and myrtle essential oils, respectively. The major constituents were described as carvacrol (81.4%) for TEO and 1,8-cineole (61%), ?-pinene (23.7%) for MEO. In its second part, the present study was conducted to evaluate the in vitro antioxidant and antimicrobial activity of both studied EOs. For this purpose, the DPPH scavenging test and disc-diffusion method was used. Results show thats both essential oils was able to reduce the stable free radical DPPH with an IC50 of 140 (TEO) and 941 mg/mL (MEO). Significant zone of lysis against all the pathogens studied. On comparing the efficiency of both EOs, T. capitatus EO exhibited higher antibacterial activity against the majority of strains and especially against Klebsiella pneumoniae (DIZ=24.2 mm). During storage, samples containing essential oils showed microbiological parameters stability better than those for the control. The sensorial evaluation shows that 0.05% of either essential oil added was best appreciated by the panelists.
112 A New Cycloheptapeptide from Zanthoxylum mezoneurispinosum Ak Assi (Rutaceae), Philomne A. Yao-Kouassi*, Catherine Caron1, Emma Ak-Assi, Agathe Martinez, Elisabeth Le Magrex-Debar, Sophie C. Gangloff and Monique Zches-Hanrot
A new cycloheptapeptide named akeassimezorine 1 and twelve known compounds: methoxychelerythrine 2, chelerythrine 3, nitidine 4, methoxyfagaridine 5, jatrorrhizine 6, tembetarine 7, N-methylatanine 8, magnoflorine 9, skimmianine 10, sesamine 11, hesperidine 12, and lupeol 13 were isolated from the roots of Zanthoxylum mezoneurispinosum Ak Assi (Rutaceae). The structures of those compounds were elucidated on the basis of one- and two-dimensional NMR and HR-ESI-MS analyses. Antibacterial activity of compound 1 was evaluated against pathogenic agents. This study constituted the first phytochemical investigation of the roots of Zanthoxylum mezoneurispinosum.
113 Reaction of 2-aminothiophenol with 2,5-dihydro-2,5-dimethoxyfuran : a facile route to a new dihydrobenzothiazine derivative, Amani Jaafar, Ali Khalaf, Fars Fars, Danielle Gre, Hassan Abdallah, Thierry Roisne, Ren Gre and Ali Hachem
Today, there is a big market for steroidal hormones as well as for their derivatives. This review traces the development in steroidal production from the first milligram-scale isolation of the products to their semi-synthesis from sapogenins, their total synthesis and finally their microbial enzymatic preparation from phytosterols.
114 Effect of thyme and myrtle leaves essential oils on the quality characteristics of cured sausage during storage, Hayet Ben Haj Koubaier, Ahmed Snoussi, Ismahen Essaidi, Soumaya Hchaichi, Nabiha Bouzouita
The aim of this work was to study the effect of adding thyme and myrtle essential oils (TEO and MEO) at different concentrations (0.05 and 1%) on the microbiological and sensorial characteristics of cured sausage during storage (21 days) at +4C. The chemical composition of essential oils, obtained by hydrodistillation, was analyzed using GC and GC-MS. Twenty and twenty three compounds were identified for thyme and myrtle essential oils, respectively. The major constituents were described as carvacrol (81.4%) for TEO and 1,8-cineole (61%), ?-pinene (23.7%) for MEO. In its second part, the present study was conducted to evaluate the in vitro antioxidant and antimicrobial activity of both studied EOs. For this purpose, the DPPH scavenging test and disc-diffusion method was used. Results show thats both essential oils was able to reduce the stable free radical DPPH with an IC50 of 140 (TEO) and 941 mg/mL (MEO). Significant zone of lysis against all the pathogens studied. On comparing the efficiency of both EOs, T. capitatus EO exhibited higher antibacterial activity against the majority of strains and especially against Klebsiella pneumoniae (DIZ=24.2 mm). During storage, samples containing essential oils showed microbiological parameters stability better than those for the control. The sensorial evaluation shows that 0.05% of either essential oil added was best appreciated by the panelists.
115 Chemical composition, antibacterial and antifungal activities of the Cedrus atlantica (Endl.) Manettiex Carrire seeds essential oil, Rachid Rhafouri, Badr Strani, Touria Zair, Mohamed Ghanmi, Abderrahman Aafi, Mohamed El Omari, Amar Bentayeb
The Atlas cedar is an endemic species of the African North Mountains. The goal for which this work was conducted is to determine the chemical composition and to study the antibacterial and the antifungal activity of the hydrodistilized essential oil from both the winged and wingless seeds of the High Atlas Cedrus atlantica (Morocco). The essential oil is analyzed by gas chromatography and gas chromatography mass spectrometry. The essential oil yields of winged as well as wingless seeds were respectively 2.6% and 3.6%.The main constituents of the cedar wingless seeds are the ?-pinene, the manool, and the bornyl acetate; whereas, the major constituents of the cedar winged seeds are the manool and the ?-pinene. The antibacterial and antifungal activities of the essential oils were tested on four bacteria, three molds and four fungi of wood rot. The fungal strains tested were revealed more sensitive to the essential oil studied than the bacterial strains.
116 Utilization of waste Tunisian palm tree date as low-cost adsorbent for the removal of dyes from textile wastewater, Sami Guiza, Khadija Ghiloufi, Final Mohamed Bagane
The removal of dyes such, as methylene blue and Congo red, from an aqueous solution is studied by adsorption Tunisian palm tree date. The equilibrium isotherm for each dye-adsorbent system was determined. The experimental results have been fitted with Langmuir and Freundlich isotherms. The maximum adsorption capacities of palm tree date are found to be 200 and 90 mg/g at dyes of methylene blue and Congo red, respectively. A comparative cost study, based on the adsorption capacity alone, has shown that the costs of the required adsorbent are 1.1%, and 1, 8%, respectively, compared with the case of commercial granular activated carbon. The Gibbs free energy values obtained confirm that the process is feasible and spontaneous ?G < 0. The negative values of ?H indicate that an exothermic chemisorption took place. The negative values of ?S suggest that the randomness decreases after adsorption.
117 Laser irradiation effects on ultrafine carbon-coated LiFePO4 using a modified solid state synthesis and olive oil as carbon source, Ghazi Ben Amor, Noureddine Amdouni, Habib Boughzala, Jean Marc Grenche
Nano-size LiFePO4/C composite was synthesized via a modified solid state reaction method. Olive oil is used as carbon source. The conventional solid state process was modified by introducing two initial steps of slurry phase blending of the ingredients and solvent removal by rotary evaporation, so as to get an intimate mixing and homogenous dispersion of reactants and conductive carbon in the sample. Both structure and morphology of the LiFePO4/C composite sample have been characterized by X-ray diffraction (XRD), Mssbauer spectrometry, transmission electron microscopy (TEM) and Raman spectroscopy. The LiFePO4/C composite exhibited a high crystallinity. The particles of synthesized LiFePO4/C were fine and homogeneous in size, with an average diameter of 100nm. Since the thermal effect of laser irradiation may possibly alter material surface, particular attention has been paid in characterizing the structure and component of the material surface by Raman spectroscopy. Electrochemical measurements show that the LiFePO4/C composite cathode delivers an initial discharge capacity of 146 mAh g?1 between 2.5 and 4.3Vat a C/10 rate (a charger rated C/10 would return the battery capacity in 10 hours).
118 Coumarin derivatives: Synthesis and cation binding properties, Olfa Naouali, Rached Frija, Wissal Elgabsi, Naceur Hamdi, Lassaad Baklouti
Coumarin derivatives were easily prepared starting from 7-hydroxy 4-methyl-2H-chromen-2-one with 40% formaldehyde and suitable secondary amines in 95% ethanol in rather good yield. The structures of all compounds were confirmed via spectroscopic techniques IR, 1H NMR, 13C NMR, mass spectra and elemental analysis. The complexing properties of the coumarin derivatives toward alkali metal, alkaline earth metal, some transition metals and some heavy metal cations have been investigated in methanol by means of UV spectrophotometry absorption and conductivity methods. Thus, the stoichiometry of the complexes formed and their stability constants were determined.
119 Alternative method to predict activity coefficients at infinite dilution of hydrocarbons in aqueous solutions, Gonzalo Astray, Jorge Morales, Miriam Gonzlez-Temes, Juan C. Mejuto, Augusto J. Magdalena
Activity coefficients at infinite dilution are important property in solute-solvent interactions. Experimental techniques show high costs, skilled labour and safety. To solve this, a neural network model with five different topological descriptors to implement different Artificial Neural Network has been implemented. The best Artificial Neural Network (5-11-8-1 topology) presents good fits for the training phase with an Average Percentage Deviation of 1.85%. Similar results have been obtained for the validation phase of the Artificial Neural Network (1.88%). The implemented Neural Networks techniques showed better results than other developed methods, around 30.70% and 24.60% for training and validation phase, respectively.
120 Alternative method to predict activity coefficients at infinite dilution of hydrocarbons in aqueous solutions, Gonzalo Astray1,2,*, Jorge Morales1, Miriam Gonzlez-Temes1, Juan C. Mejuto1 and Augusto J. Magdalena1
Activity coefficients at infinite dilution are important property in solute-solvent interactions. Experimental techniques show high costs, skilled labour and safety. To solve this, a neural network model with five different topological descriptors to implement different Artificial Neural Network has been implemented. The best Artificial Neural Network (5-11-8-1 topology) presents good fits for the training phase with an Average Percentage Deviation of 1.85%. Similar results have been obtained for the validation phase of the Artificial Neural Network (1.88%). The implemented Neural Networks techniques showed better results than other developed methods, around 30.70% and 24.60% for training and validation phase, respectively.
121 The mathematical description for the electropolymerization of furan, pyrrole and thiophene derivatives in alkaline media, Volodymyr Tkach*, Vasyl Nechyporuk and Petro Yagodynets
The electropolymerization of furan, pyrrole and thiophene in strong basic media was mathematically described. Two models for the cases of the insoluble and soluble anodes were described and analyzed by using the linear stability theory and bifurcation analysis and compared with the models for other cases of electropolymerization. The causes for the oscillatory behavior, monotonic instabilities and steady-state stability conditions were found.
122 Syntheses via phenolic oxidative coupling using crude peroxidase from Brassica juncea (L) Czern leaves and antioxidant evaluation of dimeric thymol, Yusnidar Yusuf 1,*, Budi Arman 1, Antonius H. Cahyana 2
The ability of a crude Brassica juncea (L) Czern peroxidase as green and edible catalyst for phenolic oxidative dimerization of thymol is presented. Crude peroxidase was isolated and partially purified using precipitation method with gradient concentration of ammonium sulphate and dry ice-acetone combination as temperature regulator. The crude peroxidase was then analyzed qualitatively and quantitatively using guaiacol as a model substrate and amino antypirin activity test, respectively, and the positive result was confirmed. From the phenolic oxidative reaction, dimerization of thymol was carried out under extremely mild reaction condition in aqueous medium. The product was checked by using Fourier Transform Infrared (FTIR) and Gas Chromatography-Mass Spectrometry (GC-MS). Furthermore, the biological activity test using DPPH radical scavenging method was confirmed that the dimeric thymol showed 15 times greater than monomeric thymol in term of antioxidant capacity.
123 Dispersive liquid-liquid microextraction for the preconcentration and spectrophotometric determination of copper(II) in blood serum sample using sodium diethyldithiocarbamate as the complexing agent, Reza Emamali Sabzi 1, Naimeh Mohseni 1, Morteza Bahram1,*, Mahmoud Rezazadeh Bari 2
A dispersive liquid-liquid microextraction (DLLME) process based on the complexation reaction of Cu(II) with diethyldithiocarbamate (DDTC) from aqueous solutions was investigated. The effect of various experimental parameters in the extraction such as, dispersive solvent, extracting solvent, the volume of extraction and disperser solvent, pH of the aqueous solution, ionic strength and extraction time were optimized using one variable at a time method, and the analytical charactristics of the method were obtained. Under the optimum conditions the calibration graph was linear over the range 0.01 to 0.1 ?g mL-1 of Cu(II) ion with a correlation coefficient of 0.994. The limit of detection (S/N = 3) was 8.6 10-3 ?g mL-1. Relative standard deviation (RSD) for 7 replicate determinations of 0.08 ?g mL-1 Cu(II) was 3.3%. In this work, the concentration factor of 20 and also the improvement factor of 33 were reached. The interference effect of some anions and cations was also tested. The extraction method has been successfully applied to the determination of copper in human blood serum sample.
124 Highly diastereoselective synthesis of N-substituted 4-(diethoxyphosphoryl)-pyrrolidines-3-carboxylate starting from tetraethyl methylenediphosphonate, Maha Ameur1, Acha Arfaoui1, Jihne Ben Kraem1, Salem S. Al-Deyab2 and Hassen Amri1*
This paper describes a convenient synthesis of novel series of 3,4-disubstituted pyrrolidines based on the aza-Michael addition of primary amines to 3,4-difunctionalized-1,3-diene followed by an intramolecular cyclization.
125 Investigation of the Self-Diffusion Coefficients of Trivalent Gd3+ in aqueous solutions: The Effect of Hydrolysis and nitrate ion association, Rafik Besbes * 2,3, Noureddine Ouerfelli 1, Manef Abderabba 3, Patric Lindqvist-Reis 4 and Habib Latrous 1
In recent work, we have deduced that berkelium and gadolinium, which have 4f and 5f with half-filled configurations, also display similar diffusion properties. Results, using self-diffusion coefficients to study thermodynamic properties, show very similar behavior, which is understood given their similarities in charge, ionic size, mobility, conductance, and hydration number. In this paper we undertook a study of Gd3+ as an aid for deducing the thermodynamics properties of the Bk3+ . In first part we compare magnitudes of transport (self-diffusion coefficient) of the trivalent aquo ions of Gd III for two concentrations, C1 = 2 10-4 mol.L-1, C2 = 10-3 mol.L-1 , and in perchlorate and nitrate media . In second part, we studied the variation of D with the mediums pH. Self-diffusion coefficients, D, of the trivalent f-elements aqua ions have been determined in an aqueous electrolyte support of Gd(NO3)3 and Nd(ClO4)3 and at a pH=2.5. (HNO3, HClO4 ) and at 25 C using the open-end capillary method (O.E.C.M.). The variation of D versus pH shows three zones We changed the NO3- counter ion with ClO4- ,and found that measurements must be carried in perchloric acid medium so as to avoid pairing phenomena. Using association constants between Gd3+ and NO3- , and a hydration constant, we estimated self-diffusion coefficients for Gd(NO3)2+ and Gd(OH)2+ . The results justified our choice of working at pH = 2.5 which constitute an optimum condition to avoid hydrolysis and pairing phenomena. Our results were confirmed by mobility measurements using an electro migration technique.
126 Analysis of chemical composition of high viscous oils, Irina Germanovna Yashchenko and Yury Mikhailovich Polishchuk
The spatial distribution of viscous oils which are considered as an important reserve for oil-production in future were studied on base of information from global database on oil physical and chemical properties. Changes in chemical composition of viscous oils in different basins and continents were analyzed as well. It is shown, on average, viscous oils are sulfur-bearing, low paraffin, highly resinous oils with an average content of asphaltenes and low content of the fraction boiling at 200 ?C. Study results of viscous oils peculiarities of Canada, Russia and Venezuela are given. The analysis results can be used to determine the optimal layouts and conditions of oil transportation, to improve the search methods of geochemical exploration, and to solve other problems in the oil chemistry.
127 Study of Chemical Interactions in Binary mixture water-1,4-dioxane : Neighbourhood and Associated Model Approach, Rafik Besbes* 1,3 , Noureddine Ouerfelli 2 and Manef Abderabba3
We use our results of measurements of the activities coefficients of water and 1,4-dioxane at room conditions to analyse the interactions between molecules of water and 1,4-dioxane in different mixtures. Our study is based on Neighbourhood Model Approach at liquid state in correlation with solid state to calculate molar fractions of free molecules of water and of 1,4-dioxane in pure liquid state and to deduce the composition of the various mixtures. We calculate system composition in a basis of associate model (called). This model gives good results to interpreting interactions between molecules of water and of 1,4-dioxane. Our model is inspired by resulting experimental recently published by our team, witch measurements of the enthalpy of mixture: ?mh (XD), present two maxima for molecular fraction of 1,4-dioxane XD = 0.1438 and XD = 0.7805, which correspond to arrangements between molecules of water and 1,4-dioxane of type WD3.56, and DW5.95 (D: 1,4-dioxane W: water) We use, for the study of the model suggested, a number of 4 neighbours molecules in the first shell surrounding one molecule of water and 6 neighbours molecules for one molecule of 1,4-dioxane. Our observations confirm well the results of works of many authors by different technical methods.
128 Synthesis, characterization and crystal structure of new cobalt (III) complex: [Tris(1,10-phenanthroline-?2N,N) Cobalt (III)] trinitrate monohydrate [Co(C12H8N2)3](NO3)3.H2O, Jawher Abdelhak, Saoussen Namouchi Cherni and Mohamed Faouzi Zid
We report herein the synthesis and the physicochemical characterization of a new cobalt(III) complex of formula [Co(C12H8N2)3](NO3)3.H2O. This compound has been prepared by slow evaporation at room temperature and characterized by single crystal X-ray diffraction, IR, UV-VIS spectra and thermal analysis (TG and DTA). Structural cohesion is established essentially by ?-? interactions between the rings of phenanthroline groups and intermolecular hydrogen bonds connecting the nitrate entities and uncoordinated water molecules.
129 Characterization of curcumin-nicotine interaction in cetyltrimethyammonium bromide micelle, Maurice O. Iwunze
A combination of fluorescence and UV-Vis spectrophotometric techniques were used to characterize the interaction of curcumin and nicotine in a cetyltrimethylammonium bromide (CTAB) micellar system. It is observed that in this medium curcumin and nicotine interact in a 1:1 ratio using the UV-Visible molar ration method. The fluorescence spectrophotometric technique, using the Benesi-Hildebrand equation was used to determine the association constant, Ka. The value thus obtained is 1.26 0.02 x 105 M-1 and the molar absorptivity, ?, of 2.3 0.06 x 104/M-cm. The free energy of association, ?Ga, was subsequently calculated as -29.1 kJ/mol. This vale together with the value obtained for Ka implies that the complex formed by curcumin and nicotine in this medium is not only spontaneous but it also very stable.
130 Synthesis and biological evaluation of new pyrazolo[3,4-d]pyrimidine derivatives, Asma Agrebi, Fatma Allouche, Hamadi Fetoui and Fakher Chabchoub
Several new pyrazolopyrimidine compounds were achieved from aminocyanopyarazole 1. The starting material 1 was initially coupled with orthoester at refluxed with various primary amines, ammonia, hydrazines and hydroxylamine to furnish a series of pyrazolo[3,4-d]pyrimidines. The reaction of imidate 2a-b with hydrazide derivatives led to the formation of pyrazolo[3,4-d][1,2,4]triazolo[4,3-c]pyrimidines. Some of the synthesized compounds 3a and 4c were evaluated for their anti-inflammatory, antipyretic and nociceptive activities. We start by studing the toxicity of these two molecules by measuring the corresponding DL50. The DL50 of 3a and 4c are estimated to 1333.2mg / kg and 1593.5mg / kg respectively. Pharmacological evaluation showed that compounds 3a and 4c at doses (5.5-22.2 mg / Kg, i.p) exhibited anti-inflammatory activities compared to Ibuprofen (150 mg / Kg, i.p), used as a refer ence drug. Further, our study showed that the injection of derived pyrazolopyrimidines on hyperthermic animal leads to a decrease in temperature after 1 hours of treatment compared to paracetamol used as reference. In addition, the injection of derived pyrazolopyrimidines at different doses contains a potent nociceptive activity. This effect is dose-dependent compared to aspirin.