A simple synthesis of trisubstituted quinolines through transesterification

An efficient and simple method has been reported for the synthesis of 2,3,4‐trisubstituted quinolines through zwitterion intermediate under reflux condition in presence of sulfuric acid. The formed dicarboxylate subsequently undergoes transesterification in various alcohols with good yields. Most of the synthesized compounds are newly reported characterized by spectroscopic method. J. Heterocyclic Chem., (2011).     

Studies on copolymerization of N-isopropylacrylamide with poly(ethylene glycol) methacrylate

The paper describes the preparation and characterization of cross-linked homopolymers and copolymers of N-isopropyl acrylamide (NIPAAm) with poly(ethylene glycol) methacrylate (PEGMA, M_n = 526 g/mol). Several copolymer samples were prepared by taking varying amounts of monomers i.e. NIPAAm and PEGMA in the initial feed using hydrophilic (IRGACURE-2959) and hydrophobic (DURACURE-1173) photoinitiator. In order to investigate the effect of reaction conditions, copolymers were prepared below or above the lower critical solution temperature (LCST) using water or water:ethanol (50:50) as solvent and by varying the amounts of cross-linker. Hydrogels prepared under varying reaction conditions were characterized for its swelling behaviour (using optical microscope), phase transition temperature (using DSC) and morphology (using SEM). As expected LCST increased from 35 to 39 °C as PEGMA content in copolymers increased from 1 to 20% (w/w). However, the morphology of hydrogels was found to be independent on the reaction conditions.Copolymer films having an optimum combination of swelling and performance properties were evaluated as switchable cell culture membranes. Hepatic cancer cell lines (Hep G-2) was used to study the cell growth and detachment. Cell growth and detachment were found to be dependent on the copolymer composition. Cell viability was found comparable to trypsin which also supports application of these films as cell culture membrane.     

Capillary liquid chromatography and capillary electrochromatography using silica hydride stationary phases

A hydride-based octadecyl stationary phase on both 4.0 and 1.8 microm silica particles is tested in both the capillary LC and the pressurized capillary electrochromatography (pCEC) modes. These two materials are compared to standard C18 stationary phase made by organosilanization and to the hydride material packed into a convention 4.6mm I.D. column. The performance of the capillary columns is evaluated in terms of analysis times for various mixtures as well as efficiency. Of particular interest are the differences between the LC mode where only laminar flow is present and pCEC operation where a flat electrodriven flow profile is superimposed on the parabolic pressurized flow. Differences in performance between columns packed with 4.0 and 1.8 microm particle silica are also evaluated.     

Self-assembled monolayers: solidification of carbamazepine in Form II at an interface

A self-assembled monolayer incorporating well-spaced biphenyl moieties initiates solidification of carbamazepine at its interface. A detailed analysis of the resulting crystals using X-ray powder diffraction, FTIR-ATR as well as thermomicroscopy, indicates a preference for its crystallization in trigonal (Form II) polymorph.     

Development and validation of reversed-phase column high-performance liquid chromatographic and first-derivative UV spectrophotometric methods for estimation of voriconazole in oral suspension powder

This research paper describes validated reversed-phase high-performance column liquid chromatographic (RP-HPLC) and first-derivative UV spectrophotometric methods for the estimation of voriconazole (VOR) in oral suspension powder. The RP-HPLC separation was achieved on Phenomenex C18 column (250 x 4.6 mm id, 5 microm particle size) using water-acetonitrile (40 + 60, v/v; pH adjusted to 4.5 +/- 0.02 with acetic acid) as the mobile phase at a flow rate of 1.4 mL/min and ambient temperature. Quantification was achieved with photodiode array detection at 255 nm over the concentration range of 0.1-1 microg/mL with mean recovery of 99.49 +/- 0.83% for VOR by the RP-HPLC method. Quantification was achieved with UV detection at 266 nm over the concentration range of 8-20 microg/mL with mean recovery of 99.74 +/- 0.664% for VOR by the first-derivative UV spectrophotometric method. These methods are simple, precise, and sensitive, and they are applicable for the determination of VOR in oral suspension powder.     

Bifunctional yttrium(III) and titanium(IV) NHC catalysts for lactide polymerisation

Lewis acidic yttrium(III) and titanium(IV) derivatives of anionic, metal-tethered carbenes apparently act as bifunctional catalysts for the polymerisation of D,L-lactide, using a combination of Lewis acid and base functionalities to initiate ring opening of the cyclic monomer; the alcohol- and amino-functionalised carbenes from which they derive provide models for the first insertion step, and also display metal-free polymerisation catalysis to generate polylactic acid.     

Role of surface modification of colloidal CdSe quantum dots on the properties of hybrid organic–inorganic nanocomposites

In this work, tri-octyl phosphine/tri-octyl phosphine oxide (TOPO)-capped cadmium selenide (CdSe) quantum dots (QDs) of varied sizes (5–9 nm), prepared by varying the input Cd:Se precursor ratio using chemical route, were dispersed in conducting polymer matrices viz. poly[2-methoxy, 5-(2-ethyl-hexyloxy)-1,4-phenylene vinylene] (MEH-PPV) and poly(3-hexylthiophene) (P3HT). By using a binary solvent mixture (pyridine–chloroform), homogeneous dispersion of CdSe nanocrystals in polymers (MEH-PPV, P3HT) could be realized. The properties of the resulting dispersions could be tailored by the composition and concentration of QDs in polymer. The emission and structural properties of polymer–CdSe nanocomposites are found to be dependent on the crystallite size and morphology of CdSe nanocrystallites. An effective quenching of photoluminescence emission in the polymer nanocomposite was observed for smaller CdSe quantum dots (size ∼6 nm) as compared to larger CdSe quantum dots (size ∼9 nm), thus ensuring efficient charge transfer process across the polymer–CdSe interface in the former case. The incomplete quenching, particularly for MEH-PPV:CdSe nanocomposites, could be as a result of insufficient coverage of polymers on the surface of CdSe nanocrystallites, mainly due to phase segregation for TOPO-stripped CdSe nanocrystallites. The superior morphology and optical properties of polymer nanocomposite (P3HT:CdSe QDs) could play a pivotal role for the realization of effective charge separation and transport in hybrid solar cells.     

A total reflection X‐ray fluorescence method for the determination of chlorine at trace levels in nuclear materials without sample dissolution

A total reflection X‐ray fluorescence (TXRF) method for the determination of chlorine at trace levels in nuclear fuel samples is described. Chlorine present in trace concentrations in nuclear fuel materials such as U₃O₈, (U,Pu)C, PuO₂ and Pu‐alloys was first separated from the solid matrix by pyrohydrolysis as HCl and was collected in 5 mM NaOH solution. This solution was analyzed for chlorine by TXRF spectrometry using Cl Kα analytical line excited by W Lα. Cobalt was used as internal standard. The precision for such chlorine determination was found to be within 27% (n = 4) when the analysis was carried out in air atmosphere. This could be improved to 8% by making TXRF measurement in flowing helium atmosphere. The results obtained from TXRF determinations were also compared with those obtained from ion chromatography (IC) and were in good agreement. The collection of distillate during pyrohydrolysis in NaOH helped in counterchecking loss of chlorine during TXRF sample preparation. The average deviation of TXRF‐determined values in helium‐purged TXRF measurements with IC determined values (as chloride) was 15% at a chlorine concentration level in the range of 1–70 µg/mL. Copyright © 2012 John Wiley & Sons, Ltd.     

N-methyl Benzimidazole Tethered Cholic Acid Amphiphiles Can Eradicate S. aureus-Mediated Biofilms and Wound Infections

Infections associated with Gram-positive bacteria like S. aureus pose a major threat as these bacteria can develop resistance and thereby limit the applications of antibiotics. Therefore, there is a need for new antibacterials to mitigate these infections. Bacterial membranes present an attractive therapeutic target as these membranes are anionic in nature and have a low chance of developing modifications in their physicochemical features. Antimicrobial peptides (AMPs) can disrupt the microbial membranes via electrostatic interactions, but the poor stability of AMPs halts their clinical translation. Here, we present the synthesis of eight N-methyl benzimidazole substituted cholic acid amphiphiles as antibacterial agents. We screened these novel heterocyclic cholic acid amphiphiles against different pathogens. Among the series, CABI-6 outperformed the other amphiphiles in terms of bactericidal activity against S. aureus. The membrane disruptive property of CABI-6 using a fluorescence-based assay has also been investigated, and it was inferred that CABI-6 can enhance the production of reactive oxygen species. We further demonstrated that CABI-6 can clear the pre-formed biofilms and can mitigate wound infection in murine models.