Hydrophilic interaction LC–MS/MS method to avoid endogenous interference in the analysis of 4-hydroxy isoleucine from dietary supplementation of fenugreek

4-Hydroxy isoleucine is one of the potent hypoglycemic active constituents of fenugreek seeds. A method capable of reducing biological interferences is required for bioavailability studies. An isocratic separation of 4-hydroxy isoleucine from endogenous interferences was achieved in ZIC-cHILIC column using 0.1% formic acid in water and acetonitrile (20:80, % v/v) pumped at 0.5 ml/min. Quantification was performed in multiple reaction monitoring mode using the transitions of m/z 148.1→102.1 and m/z 276.1→142.2 for 4-hydroxy isoleucine and homatropine (as internal standard), respectively. After full method validation, 4-hydroxy isoleucine levels in human plasma and commercial fenugreek formulations were determined. This method showed good linearity in the range of 50–2000 ng/mL. Intra- and interday accuracies were in the range of 90.64–109.0% and precision was <4.82% CV. The mean (SD) plasma concentration of 4-hydroxy isoleucine in healthy individuals at 2 h after oral administration of fenugreek tablet was found to be 1590 (260) ng/mL. Half of marketed formulations were found to contain <0.05% of 4-hydroxy isoleucine content. We developed a rapid hydrophilic interaction liquid chromatography–tandem mass spectrometry method for analysis of 4-hydroxy isoleucine in human plasma. This method can be applied directly to conduct the clinical pharmacokinetics studies of 4-hydroxy isoleucine in human population.     

Galactose Grafted Two-Dimensional Nanosheets as a Scaffold for the In Situ Synthesis of Silver Nanoparticles: A Potential Catalyst for the Reduction of Nitroaromatics

Two major hurdles in NP-based catalysis are the aggregation of the NPs and their recycling. Immobilization of NPs onto a 2D support is the most promising strategy to overcome these difficulties. Herein, amphiphilicity-driven self-assembly of galactose-hexaphenylbenzene-based amphiphiles into galactose-decorated 2D nanosheet is reported. The extremely dense decoration of reducing sugar on the surface of the sheets is used for the in situ synthesis and immobilization of ultrafine catalytically active AgNPs by using Tollens’ reaction. The potential of the system as a catalyst for the reduction of various nitroaromatics is demonstrated. Enhanced catalytic activity is observed for the immobilized AgNPs when compared to the corresponding discrete AgNPs. Recovery of the catalytic system from the reaction mixture by ultrafiltration and its subsequent recycling for several cycles without dropping its activity is shown. This is the first report demonstrating the in situ synthesis and immobilization of ultrafine AgNPs onto a 2D nanosheet that exhibits excellent catalytic performance for the reduction of nitroaromatics.     

High strain rate in-plane shear behavior of composites

Studies are presented on in-plane shear properties of a typical plain weave E-glass/epoxy composite under high strain rate loading. In-plane shear properties were determined with ±45 degree off-axis compression and tension tests using a split Hopkinson pressure bar apparatus. In-plane shear properties are presented as a function of axial and shear strain rates. The range of axial strain rates for off-axis compression tests was 819–2003 per sec, and for off-axis tension tests was 91–180 per sec, whereas the range of shear strain rates for off-axis compression tests was 1388–3442 per sec and for off-axis tension tests was 153–303 per sec. In general, it was observed that in-plane shear strength was enhanced at high strain rate loading compared to that at quasi-static loading. Also, it was observed that in-plane shear strength increased with increasing strain rate within the range of strain rates considered.     

Images of a spin-torque-driven magnetic nano-oscillator

We present the first space- and time-resolved images of the spin-torque-induced steady-state oscillation of a magnetic vortex in a spin-valve nanostructure. We find that the vortex structure in a nanopillar is considerably more complicated than the 2D idealized structure often-assumed, which has important implications for the driving efficiency. The sense of the vortex gyration is uniquely determined by the vortex core polarity, confirming that the spin-torque acts as a source of negative damping even in such a strongly nonuniform magnetic system. The orbit radius is ～10 nm, in agreement with micromagnetic simulations.     

Organisation of carbon nanotubes and semiconductor nanowires using lateral alumina templates

Carbon nanotubes and semiconductor nanowires have been thoroughly studied for the future replacement of silicon-based complementary metal oxide semiconductor (CMOS) devices and circuits. However, the organisation of these nanomaterials in dense transistor arrays, where each device is capable of delivering drive currents comparable with those of their silicon counterparts is still a big challenge. Here, we present a novel approach to the organisation of carbon nanotubes and semiconductor nanowires, based on the use of porous lateral alumina templates obtained by the controlled anodic oxidation of aluminium thin films. We discuss the growth of nanomaterials inside the pores of such templates and show the feasibility of our approach. Our first results point to further work on controlling the synthesis of catalyst nanoparticles at the bottom of the pores, these particles being necessary to nucleate and sustain the growth of carbon nanotubes or semiconductor nanowires. To cite this article: D. Pribat et al., C. R. Physique 10 (2009).     

Experimental studies on performance augmentation of single hole cored brick sensible heat storage system using turbulence inducers

This article presents experimental analysis on performance augmentation of a single hole cored brick regenerator using turbulence inducers. Experiments were carried out for different velocities with air as the working fluid for both charging and discharging processes of a 455 mm long aluminum regenerator with inner and outer diameters of 26 mm and 40 mm, respectively. Two numbers of turbulence inducers of 1.5 mm diameter and 13 mm long were placed in ten different combinations and the results were compared with the trials wherein no inducers were used. The mean temperature of the cored brick, exit temperature during discharge, ratio of heat transfer rate to pressure drop, and exergetic efficiencies are the characteristics that were used to study the performance of the regenerator. Placement of inducers increased the mean temperature of the regenerator and the ratio of heat transfer rate to pressure drop by about 15% and a maximum of 40%, respectively, during charging. The exit air temperature during discharge exhibited maximum improvement of 18%. Increased exergetic efficiencies of more than 10% and 5% were estimated for charging and discharging, respectively. It was also observed that the addition of inducers does not necessarily result in an increased performance, and some of the combinations in fact deteriorated the performance of the regenerator.

     

Electronic structure calculations of substitutional and interstitial hydrogen in Nb

We report the results of a theoretical study on the effects of substitutional and interstitial hydrogen atoms in niobium. We confirm that any contaminated hydrogen will occupy the interstitial site over the substitutional site in niobium. For interstitial hydrogens, the lattice deformation increases with the percentage content of hydrogen, though it is negligible at low concentrations. Substitutional hydrogens are found to prefer off-center sites in the host lattice.     

Enhancement of Electrical and Optical Properties of Sodium Bromide Doped Carboxymethyl Cellulose Biopolymer Electrolyte Films

Abstract

Biodegradable ion conducting solid polymer electrolyte films of carboxymethyl cellulose (CMC) doped with sodium bromide (NaBr) with various weight percentages were prepared by a solution casting technique. Their structural, optical and electrical properties were studied by various experimental techniques in order to understand the impact of the sodium metal salt on the biopolymer CMC’s properties. The optical parameters namely the optical bandgap energy and the refractive index, showed a significant variable variation with the metal salt concentration. The maximum dc conductivity was found to be ～5.15?×?10^?4 S cm^?1 at room temperature for the sample with 20?wt% of NaBr content in the CMC matrix. The ionic conductivity and dielectric constant in general, increased with increase in metal salt content, affirming the increase in ion concentration. The calculated transference number showed that the conductivity was mainly due to ions. The increase in conductivity was due to an increase in degree of amorphousness of the polymer upon doping, as analyzed by their XRD spectra.     

Genotoxic and Cytotoxic Properties of Zinc Oxide Nanoparticles Phyto-Fabricated from the Obscure Morning Glory Plant Ipomoea obscura (L.) Ker Gawl

The study was undertaken to investigate the antioxidant, genotoxic, and cytotoxic potentialities of phyto-fabricated zinc oxide nanoparticles (ZnO-NPs) from Ipomoea obscura (L.) Ker Gawl. aqueous leaf extract. The UV-visible spectral analysis of the ZnO-NPs showed an absorption peak at 304 nm with a bandgap energy of 3.54 eV, which are characteristics of zinc nanoparticles. Moreover, the particles were of nano-size (~24.26 nm) with 88.11% purity and were agglomerated as observed through Scanning Electron Microscopy (SEM). The phyto-fabricated ZnO-NPs offered radical scavenging activity (RSA) in a dose-dependent manner with an IC₅₀ of 0.45 mg mL⁻¹. In addition, the genotoxicity studies of ZnO-NPs carried out on onion root tips revealed that the particles were able to significantly inhibit the cell division at the mitotic stage with a mitotic index of 39.49%. Further, the cytotoxic studies on HT-29 cells showed that the phyto-fabricated ZnO-NPs could arrest the cell division as early as in the G0/G1 phase (with 92.14%) with 73.14% cells showing early apoptotic symptoms after 24 h of incubation. The results of the study affirm the ability of phyto-fabricated ZnO-NPs from aqueous leaf extract of I. obscura is beneficial in the cytotoxic application.     

Simple spectrophotometric and titrimetric methods for the determination of sulfur dioxide.

The proposed work describes a simple spectrophotmetric as well as a titrimetric method to determine sulfur dioxide. The spectrophotometric method is based on a redox reaction between sulfur dioxide and iodine monochloride obtained from iodine with chloramine-T in acetic acid. The reagent iodine monochloride oxidizes sulfur dioxide to sulfate, thereby reducing itself to iodine. Thus liberated iodine will also oxidize sulfur dioxide and reduce itself to iodide. The obtained iodide is expected to combine with iodine to form a brown-colored homoatomictriiodide anion (460 nm), which forms an ion-pair with the sulfonamide cation, providing exceptional color stability to the system under an acidic condition, and is quantitatively relatd to sulfur dioxide. The system obeys Beer's law in the range 5 - 100 microg of sulfur dioxide in a final volume of 10 ml. The molar absorptivity is 5.03 x 10(3) l mol(-1)cm(-1), with a relative standard deviation of 3.2% for 50 microg of sulfur dioxide (n = 10). In the titrimetric method, the reagent iodine monochloride was reduced with potassium iodide (10%) to iodine, which oxidized sulfur dioxide to sulfate, and excess iodine was determined with a thiosulfate solution. The volume difference of thiosulfate with the reagent and with the sulfur dioxide determined the sulfur dioxide. Reproducible and accurate results were obtained in the range of 0.1 - 1.5 mg of sulfur dioxide with a relative standard deviation of 1.2% for 0.8 mg of sulfur dioxide (n = 10).