Self‐Pillared,Single‐Unit‐Cell Sn‐MFI Zeolite Nanosheets and Their Use for Glucose and Lactose Isomerization

Single‐unit‐cell Sn‐MFI, with the detectable Sn uniformly distributed and exclusively located at framework sites, is reported for the first time. The direct, single‐step, synthesis is based on repetitive branching caused by rotational intergrowths of single‐unit‐cell lamellae. The self‐pillared, meso‐ and microporous zeolite is an active and selective catalyst for sugar isomerization. High yields for the conversion of glucose into fructose and lactose to lactulose are demonstrated.     

Facile LC‐UV methods for simultaneous monitoring of ciprofloxacin and rosuvastatin in API,formulations and human serum

An efficient, selective and cost‐effective liquid chromatographic assay was developed and validated for the simultaneous quantification of ciprofloxacin and rosuvastatin in Active Pharmaceutical Ingredients (API), pharmaceutical formulations and in human serum. The chromatographic system consisted of mobile phase methanol–water, 90:10 v/v at pH 3.0 adjusted with o‐phosphoric acid, pumped at 1.0 mL/min through a prepacked Purospher Star C18 (5 µm, 25 × 0.46 cm) column and effluent was monitored at the isosbestic point (255 nm) as well as at the λ_max of individual drugs (243 and 271 nm). The method was validated over a linear concentration range of 0.25–15 µg/mL for ciprofloxacin and 0.33–20 µg/mL for rosuvastatin (r² ≥ 0.999). The ranges of reliable response (limits of detection and quantitation) for ciprofloxacin were 3–15 and 9–45 ng/mL and 17–29 and 52–88 ng/mL, respectively, for rosuvastatin in all API, pharmaceutical formulations and human serum. Analytical recovery from human serum was >98% and relative standard deviation (RSD) was <2. The accuracies were 97.13–102.55 and 97.41–101.31% and precisions in RSD were 0.04–1.90 and 0.02–1.23% for ciprofloxacin and rosuvastatin, respectively. No matrix interferences, ion suppression/enhancement and carry‐over were detected. The total assay run time was less than 5 min. In another study, for optimum performance the detector was programmed for multiwavelength scanning at the absorption maxima of each component. Consequently, the linearity range was improved and limit of detection and quantitation values were down to 1–4 and 4–12 ng/mL for ciprofloxacin and 3–5 and 9–15 ng/mL for rosuvastatin, respectively. The validation parameters fitted ICH guidelines through the isosbestic and individual λ_max approach. The small sample volume and simplicity of preparation make this method suitable for use in human serum samples, pharmaceutical formulations, quality control, drug–drug interaction studies, clinical laboratories, drug research centers and forensic medical centers. Copyright © 2014 John Wiley & Sons, Ltd.     

Heat transfer and rheological properties of transformer oil-oxidized MWCNT nanofluid

Power transformers play a key role in power and electrical industries and thus boosting their efficiency is necessary. In this study, the effect of oxidized multi-walled carbon nanotubes on transformer oil thermophysical properties was experimentally investigated. The maximum amount of carbon nanotubes was chosen up to 0.01 mass% to assure the maximum purity of transformer oil. Heat transfer characteristics of transformer oil and nanofluids in two cases of free and forced convection were studied. Breakdown voltage, flash point, pour point, density, electrical and thermal conductivities, viscosity and shear stress, as eight important quality parameters, were determined. According to the experimental results, the Breakdown voltage decreased through concentration increasing. Electrical conductivity is not changed considerable with increasing concentration and temperature. Thermal conductivity of nanofluids and transformer oil changed with increasing temperature and concentration. Furthermore, at all concentrations and temperatures, the viscosity of the nanofluids was lower than that of transformer oil.     

A facile electrochemical method for the synthesis of new sulfonamide derivatives of potential biological significance

The electrochemical synthesis of some new sulfonamide derivatives was carried out via the electrochemical oxidation of 2,3-dihydrophthalazine-l,4-dione （1） in the presence of arylsulfinic acids （2a and 2b） as nucleophiles. The results show that, the electrogenerated phthalazine-l,4-dione （lox） participates in a Michael type addition reaction with 2a or 2b and via an EC mechanism to produce the corresponding sulfonamide derivatives. This method provides a one-pot procedure for the synthesis of new sulfonamide derivatives of potential biological significance in good yields without using toxic reagents at a carbon electrode in an environmentally friendly manner.     

Ion-solvent and ion-ion interactions of NaCl aqueous and aqueous maltose solutions at 298–323 K on viscosity data

Viscosities of sodium chloride in concentration range 1 × 10^?2 to 9 × 10^?2 ± 0.001 mol dm^?3, have been determined in aqueous and aqueous maltose systems (1.0 to 9.0 wt %) at different temperatures (298 to 323 K). The viscosity data have been analyzed by using Jones-Dole equation and the derived parameters A and B coefficients were also calculated. The data obtained from viscometric studies has been used to investigate the ion-solvent interaction and ion-ion interaction. Thermal effects on the ionic interactions were also examined under the light of transition state theory.     

Purification, characterization, kinetic properties, and thermal behavior of extracellular polygalacturonase produced by filamentous fungus Tetracoccosporium sp

For the first time, a polygalacturonase from the culture broth of Tetracoccosporium sp. was isolated and incubated at 30°C in an orbital shaker at 160 rpm for 48h. The enzyme was purified by ammonium sulfate precipitation and two-step ion-exchange chromatography and had an apparent molecular mass of 36 kDa, as shown by sodium dodecyl sulfate (SDS)-polyacrylamide gel electrophoresis. Its optimum activity was at pH 4.3 and 40°C, and the K _m and V _max values of this enzyme (for polygalacturonic acid) were 3.23 mg/mL and 0.15 μmol/min, respectively. Ag⁺, Co²⁺, EDTA, Tween-20, Tween-80, and Triton X-100 stimulated polygalacturonase activity whereas Al³⁺, Ba²⁺, Ca²⁺, Fe²⁺, Fe³⁺, Ni²⁺, Mg²⁺, Mn²⁺, and SDS inhibited it. In addition, iodoacetamide and iodoacetic acid did not inhibit enzyme activity at a concentration of 1 mM, indicating that cysteine residues are not part of the catalytic site of polygalacturonase. We studied the kinetic properties and thermal inactivation of polygalacturonase. This enzyme exhibited a t _1/2 of 63 min at 60°C and its specific activity, turnover number, and catalytic efficiency were 6.17 U/mg, 113.64 min⁻¹, and 35.18 mL/(min·mg), respectively. The activation energy (ΔE ^#) for heat inactivation was 5.341 kJ/mol, and the thermodynamic activation parameters ΔG ^#, ΔH ^#, and ΔS ^# were also calculated, revealing a potential application for the industry.     

Uptake of Tm(III) ions onto polyurethane foam from H2O - ethanol mixture containing 1-(2-pyridylazo)-2-naphthol (PAN)

Summary The sorption of microquantities of Tm(III) ions on washed polyurethane foam (PUF) from a mixture of aqueous solution and ethanol containing PAN was examined. The maximum sorption of 3.18^. 10^-6M solution of Tm(III) ions was observed at pH 8 with 30-minute equilibration time. The optimum ratio of aqueous-ethanol phase for the sorption of Tm(III) ions was found to be 3:1 v/v, respectively. The sorption rate of metal ions on PUF is followed a first order kinetics and obeyed the equation for an intra particle diffusion process. The equilibrium concentration data of Tm(III) ions could be described satisfactorily by several adsorption isotherms. The Freundlich adsorption isotherm constants 1/nand K_Fare 0.66±0.02 and (5.7±0.3)^. 10^-3mol^. g^-1, respectively. The Langmuir isotherm constants for monolayer coverage (Q) and binding strength of sorption (b) are (2.5±0.7)^. 10^-5mol^. g^-1and (1.6±0.1)^. 10⁴l^. mol^-1, respectively. The sorption capacity derived from Dubinin-Radushkevich (D-R) isotherm is (1.7±0.2)^. 10^-4mol^. g^-1and the sorption free energy (E) is 9.8±0.2 kJ^. mol^-1indicating chemisorption phenomena. The thermodynamic parameters indicate that the sorption of Tm(III) ions onto PUF is endothermic, entropy driven and spontaneous in nature.     

Synthesis and characterization of [Cu(Phca2en)(PPh3)X] (X=Cl, Br, I, NCS, N3) complexes: crystal structures of [Cu(Phca2en)(PPh3)Br] and [Cu(Phca2en)(PPh3)I]

New mixed-ligand copper(I) complexes, [Cu(Phca₂en)(PPh₃)X], [Phca₂en = N,N′-bis(β-phenylci-nnamaldehyde)-1,2-diiminoethane and X=Cl (1), Br (2), I (3), NCS (4), N₃ (5)] have been synthesized and characterized by various techniques. ¹H and ¹³C-NMR and IR spectral data of these copper(I) complexes are compared with the free ligand to elucidate some structural features. The structures of [Cu(Phca₂en)(PPh₃)Br] (2) and [Cu(Phca₂en)(PPh₃)I] (3) have been determined from single-crystal data showing that the coordination geometry around copper atom is a distorted tetrahedron. Furthermore, these Cu(I) complexes exhibit supramolecular motifs of the type multiple phenyl embraces resulting from attractive interactions between phenyl rings of PPh₃ moieties. The presence of the C–H…Cu weak intramolecular hydrogen bonds, due to the trapping of C–H bonds in the vicinity of the metal atoms, is also reported.     

MgBr2·OEt2 mediated protection of alcohols with hexamethyldisilazane: An efficient catalytic route for the preparation of silyl ethers under solvent-free conditions

Various types of alcohols and phenols were rapidly protected by hexamethyldisilazane in good to excellent yields at room temperature in the presence of catalytic amount of magnesium bromide ethyl etherate under solvent-free conditions. Good to excellent chemoselectivity was demonstrated for competitive protection of primary hydroxyls in the presence of secondary and tertiary alcohols. Highly selective protection of phenols in the presence of aromatic amines was also demonstrated successfully.     

Equilibrium and hydrolysis ofα-amino acid esters in ternary complexes of copper(II) involving glycyl-L-tyrosine

Summary Binary and ternary complexes of copper(II) with glycyl-L-tyrosine and an amino acid ester were investigated by potentiometric and spectrophotometric techniques. The kinetics of base hydrolysis of the above esters in the presence of copper(II)-glycyl-L-tyrosine complex was studied at 30°C.