High-performance liquid chromatographic enantioseparation of (R,S)-fluoxetine using Marfey's reagent and (S)-N-(4-nitrophenoxycarbonyl) phenylalanine methoxyethyl ester as chiral derivatizing reagents along with direct thin-layer chromatographic resolution and isolation of enantiomers using L-tartaric acid as mobile phase additive

Chiral assay of enantiomers of fluoxetine was achieved in pharmaceutical formulations using direct and indirect methods. L-tartaric acid was used as a mobile phase additive in thin-layer chromatography; the enantiomers were separated and isolated and were used to determine the elution order in HPLC. (R,S)-flouxetine was derivatized with (S)-N-(4-nitrophenoxycarbonyl)phenylalanine methoxyethyl ester [(S)-NIFE], Marfey's reagent and 1-fluoro-2,4-dinitrophenyl-L-methionine amide (FDNP-L-Met-NH?. The diastereomers were separated using RP-HPLC. The effect of flow rate and TFA concentration on resolution was studied. The diastereomers obtained by derivatization with FDNP-L-Met-NH? were also separated by RP-TLC.     

Sr induced modification of structural,optical and magnetic properties in Bi1−xSrxFeO3 (x = 0, 0.01, 0.03, 0.05 and 0.07) multiferroic nanoparticles

Multiferroic nanoparticles of Bi_1?xSr_xFeO₃ (x = 0, 0.01, 0.03, 0.05 and 0.07) were prepared by a facile sol–gel route and the variation of their structural, optical, dielectric and magnetic properties on strontium concentration has been studied. XRD and TEM results confirm the phase purity of the samples having high degree of crystallinity and monodispersity. The average particle size shows an exponential decline with increase in Sr concentration. A shape transformation from a multifaceted polygon to a spherical one has been observed as Sr concentration in the sample increases to 5%. In the second derivative FTIR spectra, the intensity of vibration peak at ～593 cm^?1 that is characteristic of rhombohedral BiFeO₃ is seen to decrease after Sr doping. All the samples showed typical M–H behavior of a ferromagnet with saturation magnetization achieved within an applied magnetic field of 10 kOe. The sample with 3% Sr substitution displayed saturation and remanent magnetization values 1.37 emu/g and 0.32 emu/g respectively that are highest among all the samples studied. Presence of exchange coupling produced due to interaction between the antiferromagnetic core and ferromagnetic shell is also observed in all Bi_1?xSr_xFeO₃ nanoparticles.     

Different approaches of impregnation for resolution of enantiomers of atenolol,propranolol and salbutamol using Cu(II)-l-amino acid complexes for ligand exchange on commercial thin layer chromatographic plates

Atenolol and propranolol (the β-blocking agents) and salbutamol (broncho- and vasodilator) were resolved into their enantiomers by adopting different modes of loading/impregnating the Cu(II) complexes of l-proline (l-Pro), l-phenylalanine (l-Phe), l-histidine (l-His), N,N-dimethyl-l-phenylalanine (N,N-Me₂-l-Phe), and l-tryptophan (l-Trp) on commercial precoated normal phase plates. The three different approaches were (A) using the Cu(II)-l-amino acid complex as chiral mobile phase additive, (B) ascending development of plain commercial plates in the solutions of Cu complex, and (C) using a solution of Cu(II) acetate as mobile phase additive for the commercial TLC plates impregnated with ascending development of plates in the solutions of amino acid. Spots were located using iodine vapour. The results obtained for the three methods have been compared for their efficiency and the issue of involvement of the Cu(II) cation for the best performance of the three methods has been discussed with respect to the same mobile phase. The detection limit is 0.18 μg for each enantiomer.     

Indirect enantioresolution of (R,S)‐mexiletine by reversed‐phase high‐performance liquid chromatography via diastereomerization with [(S,S)‐O,O'‐di‐p‐toluoyl tartaric acid anhydride], (S)‐naproxen and nine chiral reagents synthesized as variants of Marfey's reagent

Eleven chiral derivatizing reagents (CDRs) were used for preparation of diastereomers of (R,S)‐mexiletine containing a primary amino group in close proximity to the stereogenic center. One anhydride, namely [(S,S)‐O,O'‐di‐p‐toluoyl tartaric acid anhydride] was synthesized and (S)‐naproxen was used as such as the chiral derivatizing reagent. The other nine CDRs were synthesized by substituting one of the fluorine atoms in 1,5‐difluoro‐2,4‐dinitrobenzene with six amino acid amides and three amino acids. The diastereomers were separated by reversed‐phase high‐performance liquid chromatography. The method was validated for linearity, accuracy, limit of detection and limit of quantification. The limit of detection was found in the range of 10–30 pmol. Copyright © 2010 John Wiley & Sons, Ltd.     

Separation of Aminoglycosides by Normal- and Reversed-Phase TLC

JPC – Journal of Planar Chromatography – Modern TLC - The normal-phase (NP) and reversed-phase (RP) thin-layer chromatographic separations of aminoglycosides (streptomycin, kanamycin,...     

Synthesis,Characterization, and Antibacterial Activity of Novel (1H‐Benzo[d]imidazole‐2‐yl)‐6‐(diethylamino)‐3H‐one‐xanthene,Phenoxazine, and Oxazine

A series of novel (1H‐benzo[d]imidazole‐2‐yl)‐6‐(diethylamino)‐3H‐one‐xanthene, phenoxazine, and oxazine derivatives have been synthesized from 2‐(2′,4′‐dihydroxyphenyl) benzimidazole intermediate. Synthesized compounds 8a , 8b , 8c , 8d are fluorescent in solution, photophysical properties of compounds were studied and results revealed that compounds absorb and emit in UV–visible region with good fluorescence quantum yield. Synthesized compounds are thermally stable up to 300°C. The antibacterial activities of the synthesized compounds were studied by the well‐diffusion method. Escherichia coli (ATTC‐25922), Staphylococcus aureus (ATCC‐25923), Micrococcus (ATCC‐4698), and Bacillus subtilis (ATCC‐55422) were used to investigate the antibacterial activities.     

Nanoscale characterization of different stiction mechanisms in electrostatically driven MEMS devices based on adhesion and friction measurements

In this work, for the first time different stiction mechanisms in electrostatic micro-electromechanical systems (MEMS) switches were studied. In these devices stiction can be caused by two main mechanisms: dielectric charging and meniscus formation resulting from the adsorbed water film between the switch bridge and the dielectric layer. The effect of each mechanism and their interaction were investigated by measuring the adhesive and friction forces under different electrical stress conditions and relative humidity levels. An atomic force microscope (AFM) was used to perform force-distance and friction measurements on the nanoscale. A novel technique was proposed to measure the induced surface potential over the dielectric surface and was used to explain the obtained adhesive and friction results. The evolution of adhesive force with time was monitored in order to study the charging/discharging processes in the dielectric film. The assessment methodology is employed for application in RF-MEMS switches and could be extended to other electrostatic MEMS devices. The study provides an in-depth understanding of different stiction mechanisms, and explanation for the literature reported device level measurements for electrostatic capacitive MEMS switches.     

Role of surface roughness and lubricant film thickness in nanolubrication of sliding components in adaptive optics

Silver-coated copper particles with various silver loading were prepared by a direct liquid-to-particle conversion process in spray pyrolysis reactor system. The prepared particles were completely densified at 900°C within a residence time of 2.1 s and had core-shell structure, of which formation mechanism was proposed. The mean diameter of particles was 0.45 μm. Copper particles of 20 wt.% of silver loading were stable under air and 95% of copper remained as metallic copper even after 1 month of exposure to air. This enhanced air-stability contributed to the enhanced electrical property of conductive film obtained from the coated particles. The conductive film obtained from 15 wt.% of silver-coated copper particles had a sheet resistance of 1.2 mΩ square(-1). This low resistance resulted from the lack of oxide layer and low sintering temperature of silver layer.