A Validated chiral LC Method for the Enantiomeric Separation of Galantamine

A rapid isocratic chiral HPLC method has been developed for the separation of R-galantamine from S-galantamine. Good resolution viz. Rs > 3 between R- and S- forms of galantamine was achieved with chiralpak AD-H (250 × 4.6 mm) column using n-hexane, 20% propionic acid in isopropanol and diethyl amine in the ratio of 80:20:0.2 (v/v) as mobile phase at ambient temperature. Flow rate was kept as 0.8 mL min⁻¹ and the elution was monitored at 289 nm. This method was further used to determine the amount of R-galantamine in pure and pharmaceutical formulations of S-galantamine. This method is capable to detect and quantitate R-galantamine to the levels of 0.21 and 0.84 μg mL⁻¹, respectively. The method was validated as per International Conference on Harmonization (ICH) guidelines in terms of limit of detection (LOD), limit of quantification (LOQ), linearity, precision, accuracy, specificity, robustness and ruggedness.     

Enhanced optical and nonlinear optical responses in a polyelectrolyte templated Langmuir-Blodgett film

Optical and nonlinear optical properties like fluorescence and second harmonic generation (SHG) of molecular materials can be strongly influenced by the mode of assembly of the molecules. The Langmuir-Blodgett (LB) technique is an elegant route to the controlled assembly of molecules in ultrathin films, and complexation of ionic amphiphiles in the Langmuir film by polyions introduced in the aqueous subphase provides a simple and efficient access to further control, stabilization, and optimization. The monolayer LB film of the hemicyanine-based amphiphile, N-n-octadecyl-4-[2-(4-(N,N-ethyloctadecylamino)phenyl)ethenyl]pyridinium possessing a "tail-head-tail" structure, shows fluorescence as well as SHG response. The concomitant enhancement of both of these linear and nonlinear optical attributes is achieved through templating with the polyanion of carboxymethylcellulose. Brewster angle and atomic force microscopy reveal the influence of polyelectrolyte templating on the morphology of the Langmuir and LB films. Polarized absorption and fluorescence spectroscopy provide insight into the impact of complexation with the polyelectrolyte on the orientation and deaggregation of the hemicyanine headgroup leading to fluorescence and SHG enhancement in the LB film.     

A Validated Chiral LC Method for the Enantiomeric Separation of Cinacalcet Hydrochloride

A rapid isocratic chiral LC method has been developed for the separation of (S)-cinacalcet from (R)-cinacalcet. Good resolution with R _S  > 3 was obtained using a Chiralpak-IA column (250 × 4.6 mm, particle size 5 μm) and n-hexane, ethanol and trifluoroacetic acid as the mobile phase (95:5:0.1, v/v) at ambient temperature. Flow rate was kept at 1.0 mL min^–1 and elution was monitored by UV detection at 223 nm. This method was further used to determine the presence of (S)-cinacalcet in enantiopure pharmaceutical formulations containing (R)-cinacalcet. This method allowed for the detection and quantitation of (S)-cinacalcet of levels at 0.04 and 0.16 μg mL^–1, respectively. The method was validated following ICH guidelines.     

Mössbauer and other spectral studies of iron(II) complexes with amide-containing ligands

Summary Iron(II) complexes of the type [FeL₂X₂] (L=bidentate ligand, X=H₂O, Cl, or SCN) and [FeL₂] (L=tridentate ligand) with polydentate ligands derived from 2-(acetylamino)benzoic acid, 2-(benzoylamino)benzoic acid,2-[2-aminobenzoylamino]benzoic acid, 2-[amino-carbonyl]benzoic acid, 2-[(phenylamino)carbonyl]-benzoic acid, 2-[aminobenzoyl]benzoic acid and 2-aminobenzanilide have been synthesized and characterized by elemental analyses, conductivity, magnetic susceptibility and i.r., electronic, n.m.r., and Mossbauer spectral studies. The different modes of ligand chelation and the stereochemistry around the metal ion are discussed. The small range of isomer shift values for iron(II) complexes confirms the similar geometry for all the complexes.     

Polymer‐anchored copper(II) complex: an efficient reusable catalyst for the synthesis of propargylamines

A new, heterogeneous, polymer‐supported copper(II) complex was prepared and characterized using various techniques, including Fourier transform infrared spectroscopy, scanning electron microscopy, energy dispersive X‐ray spectroscopy, atomic absorption spectroscopy and thermogravimetric analysis. This heterogeneous copper catalyst is efficient for the synthesis of propargylamines via a three‐component coupling reaction of aldehydes, amines and alkynes. The effect of solvent on the coupling reactions was investigated. Further, the catalyst can be easily recovered quantitatively by simple filtration and reused for a minimum number of cycles without significant loss of its catalytic activity. Copyright © 2014 John Wiley & Sons, Ltd.     

Synthesis,Antimicrobial Activity,and Docking Studies of 2-Mercapto Substituted Quinazolin-4(3H)-one and Their Derivatives

An efficient, eco-friendly synthesis of a series of 2-{[3-oxo-3-(alkyl/aryl-1-yl)alkyl]thio}-3-substituted quinazolin-4(3H)-ones employing quinazolin-4(3H)-one and corresponding halo-acyl/haloalkyl as electrophiles is presented. The products were assayed for anti-bacterial activity on four bacterial species (Pseudomonas aeruginosa, Escherichia coli, Bacillus subtilis, and Staphylococcus aureus). In-silico molecular docking studies were carried out.