Rapid determination of rifaximin on dried blood spots by LC‐ESI‐MS

The use of blood spot collection cards is a simple way to obtain specimens for therapeutic drug monitoring, assessing adherence to medications and preventing toxicity in a clinical setting. A high‐throughput liquid chromatography–electrospray ionization mass spectrometric (LC‐ESI‐MS) method for determination of rifaximin on dried blood spots (DBS) was developed and validated. It involves solvent extraction of a punch of DBS followed by reversed‐phase LC on a monolithic column consisting of a silica rod with bimodal pore structure and detection by ESI‐MS. Rifampicin was used as an internal standard (IS). The run time was within 5.0 min with a very low back‐pressure at a flow rate of 0.5 mL/min. The assay was linear from 0.1 to 10 ng/mL. The mean recovery was 98.42%. The developed method is very simple, rapid and useful for clinical applications. Copyright © 2011 John Wiley & Sons, Ltd.     

Imaging of gas flow through a porous medium from a fuel cell bipolar plate by laser-induced fluorescence

The flow in a PEM fuel cell bipolar plate with a diagonal channel structure and across a carbon paper backing layer has been experimentally studied. To examine the flow inside the plate, a liquid analogue preserving dynamic similarity has been used, applying laser-induced fluorescence. This analogy, however, cannot be used to study the flow through the carbon paper, because gas and liquid surface tension are not equivalent and their flow through a porous medium will be different. For this analysis this paper proposes as a novel application, the use of acetone vapor planar induced fluorescence. With this technique, image sequences have been obtained to visualize the gas crossing the backing layer while the plate was filled with acetone-seeded air. It has been demonstrated that the pattern of the flow emerging from the diffusion layer follows that of the pressure distribution in the plate. Hence, even an apparently non-uniform velocity distribution of the reactant gases in the plate could result in an acceptable distribution over the catalyzed electrode if the pressure field is sufficiently smooth.     

Removal of selected chlorinated micropollutants by ozonation

Feasibility of ozone oxidation for the elimination of selected dissolved organic micropollutants from water and wastewaters was studied. Five organochlorine pesticides, i.e. hexachlorobutadiene, pentachlorobenzene, hexachlorobenzene, lindane, and heptachlor, were used as organic contaminants of model water. The first four of them are classified as priority hazardous substances. The oxidation treatment process was performed in a jet loop reactor. Ozone was prepared from pure oxygen. Quantification of the organochlorine pesticides in water was achieved by the gas chromatographic method after liquid-liquid extraction. Significant contribution of stripping to the removal of the investigated compounds during the ozonation treatment was also proven by the results. Effective ozonation time with regard to treatment efficiencies was 30 min, which corresponds to the ozone input of 317 mg per liter of active volume of the ozonation reactor. Single power law kinetic models were used to describe experimental data and kinetic parameters were estimated. The best fit of the experimental degradation data of all studied pollutants was obtained by the second order kinetic model. It can be concluded, based on the results obtained, that the applied ozonation process is a promising procedure for the removal of the investigated pesticides from aquatic environment.     

An Efficient One-Pot Synthesis of 2,3-Dialkyl-1,1-Diethyl-1-(Acetylamino)-3-(1,1,1-Triphenylphosphanilidene)-1,1,2,3-Propanetetracarboxylates and Their Temperature-Dependent NMR Spectra

Abstract

Stable crystalline phosphorus ylides of 1,1-diethyl 2,3-dimethyl 1-(acetylamino)-3-(1,1,1-triphenylphosphanilidine)-1,1,2,3-propanetetracarboxylates were obtained in excellent yields from the 1:1:1 addition reaction between triphenylphosphine and dialkyl acetylenedicarboxylates in the presence of diethyl acetamidomalonate as a CH-acid. These stable ylides exist in solution as a mixture of two geometrical isomers (E and Z) as a result of restricted rotation around the carbon–carbon partial double bond resulting from conjugation of the ylide moiety with the adjacent carbonyl group on the nuclear magnetic resonance (NMR) time scale at ambient temperature. The dynamic effects in the ylide moieties were investigated by ¹H NMR spectra.

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

High-performance supercapacitors based on an ionic liquid-derived nanofibrillated mesoporous carbon

This article reports the superior specific capacitance, energy, and power density of a nanofibrillated mesoporous carbon derived from an ionic liquid source (IFMC). It was concluded that high specific capacitance and good electrical conductivity were originated from contribution of nitrogen content of IFMC, also the interesting nanofibrillated structure. A specific capacitance of 235 F g^?1 at a high discharge current of 5 A g^?1 was estimated for IFMC-based electrode which is higher than the most reported capacitance for carbon materials. An excellent performance of the nanofibrillated mesoporous carbon along with proper concentration of nitrogen constituent in the carbonaceous framework is indicative for important effects of tuning the carbon nanostructure for energy storage applications.     

A new megastigmane glycoside, phoenixoside A, from Phoenix dactylifera

A new megastigmane glycoside, phoenixoside A (1), has been isolated from the n-butanol--soluble fraction of seeds of Phoenix dactylifera. The structure was characterized as (6S,7Z,9R)-hydroxy-3-oxo-ionol-9-O-beta-D-glucopyranosyl-(1" --> 6')-beta-D-glucopyranoside on the basis of 1D and 2D NMR spectroscopy, high-resolution mass spectrometry, and CD spectroscopy.     

Effect of Nickel Distributions Embedded in Amorphous Carbon Films on Transport Properties

Electrical properties of C/Ni films are studied using four mosaic targets made of pure graphite and stripes of nickel with the surface areas of 1.78,3.21,3.92 and 4.64%.The conductivity data in the temperature range of400–500 K shows the extended state conduction.The conductivity data in the temperature range of 150–300 K shows the multi-phonon hopping conduction.The Berthelot-type conduction dominates in the temperature range of 50–150 K.The conductivity of the films in the temperature range about 50 K is described in terms of variable-range hopping conduction.In low temperatures,the localized density of state around Fermi level(F)for the film deposition with 3.92% nickel has a maximum value of about 56.2×10~(17)cm~(-3)eV~(-1) with the minimum average hopping distance of about 3.43 × 10~(-6) cm.     

Gap States of ZnO Thin Films by New Methods:Optical Spectroscopy,Optical Conductivity and Optical Dispersion Energy

The optical reflectance and transmittance spectra in the wavelength range of 300–2500 nm are used to compute the absorption coefficient of zinc oxide films annealed at different post-annealing temperatures 400, 500 and 600°C.The values of the cross point between the curves of the real and imaginary parts of the optical conductivity ɑ_1 and ɑ_1 with energy axis of films exhibit values that correspond to optical gaps and are about 3.25–3.3 eV. The maxima of peaks in plots dR/dλ and dT/dλ versus wavelength of films exhibit optical gaps at about 3.12–3.25 eV.The values of the fundamental indirect band gap obtained from the Tauc model are at about 3.14–3.2 eV. It can be seen that films annealed at 600°C have the minimum indirect optical band gap at about 3.15 eV. The films annealed at 600°C have Urbach's energy minimum of 1.38 eV and hence have minimum disorder. The dispersion energy d of films annealed at 500°C has the minimum value of 43 eV.     

Laceioside,a new cycloartane saponin from Astragalus tephrosioides Boiss. var. lacei (Ali) Kirchoff.

Phytochemical investigation of the aerial parts of Astragalus tephrosioides Boiss. var. lacei (Ali) Kirchoff. (Family Fabaceae) resulted in the isolation of a new cycloartane glycoside laceioside (1). The structure of the previously undescribed compound 1 was established as 16β-acetyloxy-3-O-β-d-glucopyranosyloxy-cycloartan-11α,24ξ, 25-triol. The structure elucidation of compound 1 was based primarily on 1D and 2D-NMR techniques including ¹H and ¹³CNMR spectra, DEPT and by 2D COSY, HSQC and HMBC experiments.