Synthesis and characterization of polyaniline–zirconium dioxide and polyaniline–cerium dioxide composites with enhanced photocatalytic degradation of rhodamine B dye

For the first time, chloroform and 2-butanol were used as solvent systems for the preparation of ZrO₂–PANI and CeO₂–PANI composites. Solubility of the synthesized composites was studied in chloroform, N-methyl-2-pyrrolidinone (NMP), and in mixture of toluene?+?2-propanol (2:1). XRD and cyclic voltammetry data showed that the ZrO₂–PANI and CeO₂–PANI composites possess both crystalline and amorphous domains indicating some sort of conductivity. TGA results showed that ZrO₂–PANI composite have a better thermal stability than pure PANI; however, CeO₂–PANI composite has lower thermal stability than pure PANI. The conjugated unsaturated structure of PANI is responsible for the enhanced photocatalytic properties of ZrO₂–PANI and CeO₂–PANI. Photocatalytic results showed that, at photolysis time of 60 min, rhodamine B (RhB) dye was degraded up to 34 and 35% by ZrO₂–PANI and CeO₂–PANI, respectively. The degradation products of RhB were quantified by LC–MS and GC–MS, and accordingly, a detailed pathway was proposed.     

Carbon Paste Electrode Modified with ZrO<Subscript>2</Subscript> Nanoparticles and Ionic Liquid for Sensing of Dopamine in the Presence of Uric Acid

A novel carbon paste electrode modified with ZrO₂ nanoparticles and an ionic liquid (n-hexyl-3- methylimidazolium hexafluorophosphate) was fabricated. The electrochemical study of the modified electrode, as well as its efficiency for simultaneous voltammetric oxidation of dopamine and uric acid is described. The electrode was also employed to study the electrochemical oxidation of dopamine and uric acid, using cyclic voltammetry, chronoamperometry and square wave voltammetry as diagnostic techniques. Square wave voltammetry exhibits linear dynamic range from 1.0 × 10^?6 to 9.0 × 10^?4 M for dopamine. Also, square wave voltammetry exhibits linear dynamic range from 9.0 × 10^?6–1.0 × 10^?3 M for uric acid. The modified electrode displayed strong function for resolving the overlapping voltammetric responses of dopamine and uric acid into two well-defined voltammetric peaks. In the mixture containing dopamine and uric acid, the two compounds can be well separated from each other with potential difference of 155 mV, which is large enough to determine dopamine and uric acid individually and simultaneously. Finally, the modified electrode was used for determination of dopamine and uric acid in real samples.     

Method Development for Determination of Antibiotic Drugs Using Newly Prepared <Emphasis Type="Italic">p</Emphasis>-Morpholinomethylcalix[4]arene Mesoporous Silica-Based HPLC Column

Mesoporous materials are described by their relatively high surface areas and pore volumes. They possess uniform channels within nanometer range. These materials have numerous applications in catalysis, separation and many other fields. The qualitative and quantitative determination of antibiotic drugs, i.e., ciprofloxacin and cefixime has clinical and analytical importance due to their broad spectrum of antimicrobial activity and stability. Both antibiotic drugs are orally active and have excellent activity against different pathogens. It is for the first time that we have developed an analytical method for the simultaneous analyses of both drugs using a newly developed p-morpholinomethylcalix[4]arene (p-MC4) mesoporous silica-based HPLC column (15?×?3 mm I.D.). Furthermore, separation of these two components was carried out using isocratic elution of methanol and 0.1% aqueous formic acid (70:30 v/v) with flow rate of 1 ml min^?1 at retention time of 2.71 and 4.21 min and retention factor 1.85 and 1.19 for ciprofloxacin and cefixime, respectively; while total run time was 5 min. The developed method was repeatable with a relative standard deviation (RSD) of 0.90–2.08% for antibiotic drugs. The limits of detection and quantification of ciprofloxacin and cefixime were obtained within the range of 0.152–0.801 and 0.40–1.23 µg mL^?1, respectively. The method is highly applicable, rapid, simple, very reproducible and accurate for the separation and determination of antibiotic drugs.     

Synthesis of some heterocyclic compounds derived from indole as antimicrobial agents

Recently, indoles are considered interesting heterocyclic compounds due to their wide range of biological activities such as antimicrobial activity. Herein, some new indole derivatives containing heterocyclic moieties were synthesized using 3-chloro-1H-Indole-2-carbaldehyde (1) as a starting material, then allowed to react with compounds containing active methylene under Knoevenagel condensation and afforded the corresponding compounds (2, 3, 9). Also, the compound (1) when allowed to react with hydrazine derivatives gave the corresponding thiosemiccarbazone, semicarbazone, and hydrazone derivatives (4, 5, 6). Reaction of thiosemicarbazone derivatives with α-halognated carbonyl compounds gave the thiazolyl indole derivatives (10, 12a–b). Cyclic chalcones (11a–c) were obtained when compound (10) reacted with different aromatic aldehydes. The structures of all new synthesized compounds were confirmed on the basis of spectral analysis, IR, 1H NMR, 13C NMR, and MS spectroscopy. All synthesized compounds were evaluated for their antimicrobial activity. Compounds (2, 5, 7, 8, 11a, 12a) showed high antibacterial activity and compounds (3, 6, 9, 10, 11a, 12a) showed high antifungal activity.     

Microwave-assisted asymmetric ring opening of meso-epoxides with aromatic amines catalyzed by a Ti-S-(−)-BINOL complex

Catalytic asymmetric ring opening of cyclohexene oxide and meso-stilbene oxide with anilines was catalyzed by a Ti-(S)-(−)-BINOL complex to afford β-amino alcohols in high yield (up to 95%) and good enantioselectivities (ee up to 55%) under microwave irradiation. The reaction using a microwave was found to be 10 times faster than traditional oil-bath heating with retention of enantioselectivity.     

Studies with Heterocyclic β‐Enaminoniriles: A Simple Route for the Synthesis of Polyfunctionally Substituted Thiophene,Imidazo[1,2:1′,6′]pyrimido[5,4‐b]thiophene and Thieno[3,2‐d]pyrimidine Derivatives

Reaction of 3,5‐diaminothiophene‐2‐carbonitrile derivatives 3a‐c with ethoxycarbonylmethyl isothiocyanate and/or N‐[bis(methylthio)methylene]glycine ethyl ester led to formation of 7‐substituted‐8‐amino‐5‐thioxo‐6H‐imidazo[1,2:1′,6′]pyrimido[5,4‐b]thiophene‐2(3H)‐one derivatives 6a‐c and 7‐substituted‐8‐amino‐5‐(methylthio)imidazo[1,2:1′,6′]pyrimido[5,4‐b]thiophene‐2(3H)‐one 7a‐c , respectively. Also, the synthetic potential of the β‐enaminonitrile moiety in 3a‐c has been explored; it proved to be a promising candiate for the synthesis of 1,6‐disubstituted‐2,4‐diamino‐7,8‐dihydro‐8‐oxopyrrolo[1,2‐a]thieno[2,3‐e]pyrimidine derivatives 10a‐f and pyrido[2′,3′:6,5]pyrimido[3,4‐a]benzimidazole derivatives 12a,b .     

Conductimetric Studies of Charge Transfer Complexes of p‐Chloranil with Some Alicyclic Amines in Polar Media

The stoichiometry of charge‐transfer complexes which ionise in polar media has been studied by conductimetric titration technique in the systems morpholine‐p‐chloranil (CA), piperidine‐CA and pyrrolidine‐CA in three different polar solvents namely N,N‐dimethylformamide, acetonitrile and dimethylsulfoxide at different temperatures of 10, 15, 18, 20, 25 and 30 °C. The stoichiometric ratios of these complexes were found to vary from 1:1 to 1:4 (acceptor: donor) depending on the system, temperature and solvent used. The ασ_M‐values of these complexes have been reported. The effect of solvents, temperatures and types of electron donors on the σ_P‐values has been examined.     

RECOVERY OF VIRAL CAPACITY IN IRRADIATED EXPONENTIALLY GROWING CELLS

Exponentially growing cells of the PtK-2 line (ATCC No. CCL56, from the marsupial Potorous tridactylus) require protein and RNA synthesis in a limited period following UV-radiation damage for optimal recovery as colony formers [Overberg et al. (1988) Mutat. Res. 194, 83-92]. Overall behavior suggests the operation of damage-induced recovery processes. The capacity of confluent cell monolayers for infection with unirradiated herpes simplex virus 1 (HSV-1) is sharply reduced by UV-irradiation. We have followed capacity changes in exponentially growing cells after irradiation and varying amounts of photoreactivation by means of an infectious center assay. These changes closely parallel changes of colony formation. Spontaneous recovery of capacity in the dark occurs over approximately the same time period that the UV sensitivity of colony formation depends on macromolecular synthesis. The effect of photoreactivation is complementary rather than additive to this recovery, suggesting that the dark recovery in this period concerns pyrimidine dimers in cell DNA.     

Polarographic Determination of Famotidine through Complexation with Nickel(II) Chloride

The present investigation describes the development of a sensitive, rapid polarographic method for the determination of famotidine in pure form and in certain dosage forms. The proposed method depends upon studying the polarographic activity of Nickel(II)‐famotidine complex in Britton Robinson buffer over the pH range 4–8 and its usefulness in the analysis of famotidine using direct current (DC_t), differential pulse (DPP), and alternating current (AC_t) polarography. The different experimental parameters affecting the cathodic waves were carefully investigated and optimized. Moreover, to check the validity of the proposed method, the standard addition method was applied by adding famotidine to the previously analyzed tablets. The recovery of the drug was calculated by comparing the concentration obtained from the spiked mixtures with those of the pure drug. The results of analysis of commercial tablets and the recovery study suggested that there is no interference from any excipients, which are present in tablets. Statistical comparison of the results was performed with regard to accuracy and precision using student's t‐test and F‐ratio at 95% confidence level. There is no significant difference between the comparison and proposed method with regard to accuracy and precision.