A comparative study of complexation of enalapril with α-, β- and γ-cyclodextrins in aqueous medium: structure elucidation of inclusion complexes using NMR spectroscopic and molecular mechanics methods

Structural studies of complexes of enalapril maleate with α-, β- and γ-cyclodextrins were carried by NMR spectroscopy and computational methods. The formation of complexes of enalapril with all the three cyclodextrins was established by chemical shift changes observed in the cavity protons of cyclodextrins in the presence of enalapril maleate. The stoichiometry of the complexes was determined to be 1:1 by ¹H NMR titrations studies using Scott’s method. Intermolecular cross peaks observed in the 2D ROESY spectra of mixtures of enalapril maleate with three cyclodextrins helped in establishing the probable structures of these inclusion complexes which were supported by molecular mechanics (MM2) studies. Enalapril forms 1:1 inclusion complex with all the studied cyclodextrins through aromatic ring. The mode of approach of aromatic ring to the α-cyclodextrin cavity was found to be different from those of β- and γ-cyclodextrins, which were identical.     

An investigation of dielectric resonator antenna produced from silicon (100) enhanced by strontium doped-barium zirconate films

Dip-coated Ba_1−x Sr _x ZrO₃ thick films with different Ba/Sr ratios (x = 0.0, 0.1, 0.3, 0.5, 0.7 and 0.9) were fabricated on Si (100-orient) substrate at a low temperature of 800 °C via the sol gel method. The experimental results show that dielectric resonator (DR) properties of Ba_1−x Sr _x ZrO₃ films depend on the different Ba/Sr ratios. For structural characterization, the X-ray analysis revealed that phase transformation was affected by the increase in Sr concentrations for heat treatment at 800 °C. The films were crystalline and of single phase. The thickness of one BSZ film is around 1.259 μm when measured using the field emission scanning electron microscope. The BSZ film’s surface morphology as indicated by the atomic force microscopy showed the mean grain size to be in the range of 2.56 to 94.34 μm, and the surface roughness (RMS) was recorded to be between 2.35 to 19.64 nm. The dielectric resonator (DR) properties were measured using a network analyzer. By introducing Ba_1−x Sr _x ZrO₃ (BSZ) films on the high dielectric Si (100-orient) substrate, better frequency stability was achieved i.e. within the range of 8–10 GHz. Measured results show that Si (100-orient) DRA has a 10 dB impedance bandwidth of 4.11% at 9.34 GHz and the BSZ improved this to 11.34% with x = 0.7 at 9.15 GHz. The radiation pattern was observed to be stable throughout the operating frequency and holds good potential for DR applications.     

Asymmetric Hydrolytic Kinetic Resolution with Recyclable Macrocyclic CoIII–Salen Complexes: A Practical Strategy in the Preparation of (R)‐Mexiletine and (S)‐Propranolol

A chiral cobalt(III) complex ( 1 e ) was synthesized by the interaction of cobalt(II) acetate and ferrocenium hexafluorophosphate with a chiral dinuclear macrocyclic salen ligand that was derived from 1R,2R‐(?)‐1,2‐diaminocyclohexane with trigol bis‐aldehyde. A variety of epoxides and glycidyl ethers were suitable substrates for the reaction with water in the presence of chiral macrocyclic salen complex 1 e at room temperature to afford chiral epoxides and diols by hydrolytic kinetic resolution (HKR). Excellent yields (47 % with respect to the epoxides, 53 % with respect to the diols) and high enantioselectivity (ee>99 % for the epoxides, up to 96 % for the diols) were achieved in 2.5–16 h. The Co^III macrocyclic salen complex ( 1 e ) maintained its performance on a multigram scale and was expediently recycled a number of times. We further extended our study of chiral epoxides that were synthesized by using HKR to the synthesis of chiral drug molecules (R)‐mexiletine and (S)‐propranolol.     

Micro-Raman observation on the HPO4(2-) association structures in an individual dipotassium hydrogen phosphate (K2HPO4) droplet

A single K(2)HPO(4) droplet with size of ～50 μm on a Teflon substrate was forced to enter into the supersaturated state by decreasing the relative humidity (RH), allowing accurate control over the concentration of the solute within a droplet of a nanogram. The K(2)HPO(4) solutions from dilute (0.1-1.0 mol·L(-1) bulk) to concentrated state (a droplet from RH 98.2% to 25.1%) were studied through micro-Raman spectroscopy in the spectral region of about 200-4000 cm(-1). The area ratio between the water stretching band to the sum of the ν(1)-PO(3), ν(2)-POH, and ν(4)-PO(3) bands of the HPO(4)(2-) at various RHs was used to describe the dehydration behavior of a microsized single K(2)HPO(4) droplet in dehumidifying process. The peak position of the v(1)-PO(3) band for the 1 mol·L(-1) bulk solution appeared at 991 cm(-1) and moved to 986 cm(-1) at 98.2% RH, to 978 cm(-1) at 70.2% RH, and then to 964 cm(-1) at 30.0% RH for a droplet, accompanying an increase of the full width at half-height (fwhh) of this peak from 16.3 to 17.2, 22.2, and then to 24.2 cm(-1), indicating transition of the HPO(4)(2-) anions from monomers to dimers/trimers/oligomers and then to polyanions with chain structures in the K(2)HPO(4) solutions. After 25.1% RH, the solid was proved to be K(2)HPO(4)·3H(2)O according to the Raman spectral features. Furthermore, the O-H stretching envelope of a K(2)HPO(4) droplet showed that the intensity ratios of the strong hydrogen bonding component (3255 cm(-1)) to the weak one (3417 cm(-1)) and the cage-like water (2925 cm(-1)) to the weak one (3417 cm(-1)) were sensitive to the HPO(4)(2-) association structures, which can be used to understand the effects of dimers/trimers/oligomers and chain structures of the HPO(4)(2-) associations on the hydrogen bonding of water molecules.     

Synthesis,characterization and impregnation of lead sulphide semiconductor nanoparticles on polymer matrix

Lead sulphide nanoparticles were prepared using a precursor and dual sources methods. The composites were fabricated by stabilizing chemically synthesized semiconductor PbS nanocrystals into laurylmethacrylate and ethyleneglycol dimethacrylate matrix in the presence of tri-n-octylphosphine. PbS nanocrystals were dispersed in toluene as a compatible medium for the polymerization and cross-linking of poly laurylmethacrylate networks. The nano-sized particles and polymer composites were characterized by XRD and TEM. Possible formulations and incorporation of these PbS nanoparticles in polymer matrix have been discussed. The reported lead sulphide nanoparticles into tailered polymeric system show greater uniformity and stability.     

Spectrophotometric study of stability constants of cimetidine–Ni(II) complex at different temperatures

Cimetidine, a histamine H₂-receptor, has a structure which enables it to act as a chelating agent. The formation of nickel(II) complex with cimetidine has been studied spectrophotometrically at an absorption maximum of 622 nm at different temperatures. The data show that nickel(II) and cimetidine combine in the molar ratio of 1:2. The stability constants of the complex were calculated to be 1.40–2.4 × 10⁸ by continuous variation method and 1.24–2.4 × 10⁸ by mole ratio method at 25 and 40 °C, respectively. The immediately formed complex shows stability with respect to time and temperature.     

A Method of Computing Accurate 3D Fields of a Quadrupole Mass Filter and Their Use for Prediction of Filter Behavior

A method is described that enables the three-dimensional fields of a simple quadrupole mass filter (QMF) to be determined to a high accuracy. The technique produces accurate field values in the fringe field region as well as in the center of the filter. Using fields obtained typical filter performance is determined and shown to differ from that predicted when fringe fields are ignored. The computed performance shows features obtained experimentally and displays more complex variation with ion mass and other parameters than when fringe fields are ignored.     

Hybrid ZnO/SWNT Nanostructures Based Gas Sensor

Zinc oxide (ZnO) nanoparticles decorated single walled carbon nanotubes (SWNTs) were electrochemically synthesized where the deposition conditions were systematically explored to tailor the size, density, and microstructure of the ZnO nanoparticles and correlated to the gas sensing performance. Room temperature conductometric detection of various analytes including CO, CO₂, NO₂, NH₃, SO₂, H₂S with ZnO/SWNT hybrid nanostructures demonstrated uncharacteristic selectivity towards H₂S with little to no response for the other analytes examined. Optimal ZnO/SWNTs gas sensor devices showed a significantly increased in H₂S sensitivity over unfunctionalized SWNT networks (i.e. 4.96 % per ppm_V vs. 0.225 % ppm_V) with a lower detection limit in the ppb range. Additionally, the H₂S sensing performance was greatly improved by enhancing the crystallinity of ZnO nanoparticles.     

Unravelling the specific site preference in doping of calcium hydroxyapatite with strontium from ab initio investigations and Rietveld analyses

Strontium can be substituted into the calcium sublattice of hydroxyapatite without a solubility limit. However, recent ab initio simulations carried out at 0 K report endothermic nature of this process. There is also striking discrepancy between experimentally observed preference of Sr doping at Ca-II sites and the first principles calculations, which indicate that a Ca-I site is preferred energetically for the Sr substitution. In this paper we combine insights from Density Functional Theory simulations and regular configurational entropy calculations to determine the site preference of Sr doping in the range of 0-100 at% at finite temperatures. In addition, samples of Sr-HA are synthesized and refinement of the relevant structural information provides benchmark information on the experimental unit cell parameters of Sr-HA. We find that the contribution of the entropy of mixing can efficiently overcome the endothermic excess energy at a temperature typical of the calcining step in the synthesis route of hydroxyapatite (700-950 °C). We observe that the most preferential substitution pattern is mixed substitution of Sr regardless of the concentration. For a wet chemical method, carried out at a moderate temperature (90 °C), the mixed doping is still slightly favourable at higher Sr-concentrations, except the range at 20% Sr, where Site II substitution is not restricted energetically and equally possible as the mixed doping. We observe a close correspondence between our theoretical results and available experimental data. Hence it should be possible to apply this theory to other divalent dopants in HA, such as Zn(2+), Mg(2+), Pb(2+), Cu(2+), Ba(2+), Cd(2+) etc.     

Antimicrobial activity of the methanolic bark extract of Holarrhena pubescens (Buch. Ham), its fractions and the pure compound conessine

The antimicrobial activity of the methanolic extract of the bark of Holarrhena pubescens, its fractions, and conessine, a steroidal alkaloid, was determined against various bacteria and fungi using the agar diffusion method. They were all found to possess significant activity against some of the bacteria tested. The alkaloidal fraction and conessine also exhibited marginal activity against some of the fungi tested. The minimum inhibitory concentration (MIC) value of conessine was determined against various bacteria, and the highest activity was seen against Micrococcus luteus ATCC 9341 (MIC: 15.6?μg per disc).