1H, 13C and 15N NMR assignments for N‐ and O‐acylethanolamines,important family of naturally occurring bioactive lipid mediators

The complete ¹H, ¹³C and ¹⁵N NMR signal assignments of some N‐ and O‐acylethanolamines, important family of naturally occurring bioactive lipid mediators, were achieved using one‐dimensional and two‐dimensional experiments (gs‐HMQC and gs‐HMBC). Copyright © 2012 John Wiley & Sons, Ltd.     

Complexes of osmium (III) obtained from OsO4 and ethylenethioureas. A kinetic study of the reduction in HClO4 solutions

Summary OsO₄ reacts with imidazolidine-2-thione and itsN-methyl andN-ethyl derivatives in acidified 11 vol. H₂O:EtOH to give [OsL₆]³⁺. Complexes obtained in the presence of HClO₄ or HBF₄ have been isolated as crystals and characterized by elemental analysis, i.r. spectroscopy and magnetic measurements.All the ligands bind the metal through the sulphur atom and the magnetic measurements are consistent with low spin osmium(III). The kinetics of [OsL₆]³⁺ formation has been followed spectrophotometrically. Thepseudo-first order rate constants are linear both with respect to the acid and the ligand concentrations, indicating that the kinetically significant process involves one proton and one molecule of the ligand. A comparison of these results with those obtained for the analogous reaction with thiourea is reported.     

Asymmetric Landau-Zener tunneling in a periodic potential

Using a simple model for nonlinear Landau-Zener tunneling between two energy bands of a Bose-Einstein condensate in a periodic potential, we find that the tunneling rates for the two directions of tunneling are not the same. Tunneling from the ground state to the excited state is enhanced by the nonlinearity, whereas in the opposite direction it is suppressed. These findings are confirmed by numerical simulations of the condensate dynamics. Measuring the tunneling rates for a condensate of rubidium atoms in an optical lattice, we have found experimental evidence for this asymmetry.     

Development of a Validated Stability-Indicating LC Assay and Stress Degradation Studies of Linezolid in Tablets

This paper describes the validation of an isocratic LC method for the assay of linezolid in tablets. Validation parameters such as linearity, precision, accuracy, specificity, limit of detection, limit of quantitation and robustness were determined. LC was carried out by reversed phase technique on an RP-18 column with a mobile phase composed of 1% acetic acid:methanol:acetonitrile (50:25:25, v/v/v). Linezolid and your combination drug product were exposed to acid, base, oxidation, dry heat and photolytic stress conditions. A linear response (r > 0.9999) was observed in the range of 8.0–20.0 μg mL⁻¹. The retention time of linezolid was 4.6 min. The method showed good recoveries and intra- and inter-day relative standard deviations were less than 1.0%. The LOD and LOQ were 0.21 and 0.63 μg mL⁻¹, respectively. The developed LC method for determination of related substances and assay determination of linezolid can be used to evaluate the quality of regular production samples. It can also be used to test the stability samples of linezolid.

     

Optofluidic integrated cell sorter fabricated by femtosecond lasers

The main trend in optofluidics is currently towards full integration of the devices, thus improving automation, compactness and portability. In this respect femtosecond laser microfabrication is a very powerful technology given its capability of producing both optical waveguides and microfluidic channels. The current challenge in biology is the possibility to perform bioassays at the single cell level to unravel the hidden complexity in nominally homogeneous populations. Here we report on a new device implementing a fully integrated fluorescence-activated cell sorter. This non-invasive device is specifically designed to operate with a limited amount of cells but with a very high selectivity in the sorting process. Characterization of the device with beads and validation with human cells are presented.     

Microwave-assisted synthesis of 4-quinolylhydrazines followed by nickel boride reduction: a convenient approach to 4-aminoquinolines and derivatives

Nickel(II) chloride/sodium borohydride combination was employed for the reduction of 4-hydrazinoquinoline derivatives to the corresponding anilines. This reductive protocol was efficiently applied for the reductive cleavage of monosubstituted hydrazines. We described herein the microwave-assisted synthesis of 4-hydrazinoquinolines, which furnished a high yielding and rapid two-step procedure for the synthesis, under mild conditions, of 4-aminoquinolines as antimalarial precursors.     

N-C bond cleavage in the acid-catalyzed decomposition of some dithio- and diselenocarbamates : A kinetic investigation of dithiocarbamate decomposition in benzene and methanol

The acidic decomposition of some dithiocarbamic internal salts in MeOH and in benzene has been carried out by UV spectrophotometric measurements under pseudo-first order conditions. In both solvents the reaction is a first order with respect to the substrate and the HCl concentration. A mechanism with two consecutive irreversible steps is proposed in benzene and the results are compared with the diselenocarbamates under the same conditions. In methanol a reversible first stage has been proposed. A general conclusion on the kinetic behaviour of dithio- and diselenocarbamates in solvents at different dielectric constants has been suggested.     

A simple approach for coupling liquid chromatography and electron ionization mass spectrometry

A miniaturized, aerosol based interface for directly coupling a liquid chromatograph with a mass spectrometer is presented. The interface is entirely within the electron ionization (EI) source of the mass spectrometer and no additional, external devices are needed. This simple and effective approach exploits micro-flow nebulization technology providing a new interface suitable for a variety of applications of environmental and biological interest. The new interface provides necessary linearity, ruggedness, sensitivity, and reproducibility of response for trace level analysis, and readily interpretable mass spectra for unambiguous identification of unknown compounds of small to medium molecular weight.     

Identification of levoglucosan and related steroisomers in fog water as a biomass combustion tracer by ESI-MS/MS

A conspicuous fraction of the water soluble organic compounds (WSOC) in fog and fine aerosol samples is composed by monosaccharide anhydrides, such as levoglucosan and its stereoisomers, galactosan and mannosan. Levoglucosan is produced exclusively during wood combustion processes, making it a very useful tracer for plant combustion emissions in the atmosphere. This paper describes a new experimental approach, based on electrospray-tandem mass spectrometry (ESI-MS/MS), for the identification of levoglucosan in fog water samples. The analytical method proposed allows to identify the specific sugar anhydrides directly in the liquid phase without the need of any derivatization process.