LC-MS–MS Determination of Pregabalin in Human Plasma

A rapid, sensitive and specific method to quantify pregabalin in human plasma using metaxalone as the internal standard is described. Sample preparation involved simple protein precipitation by using acetronitrile as solvent. The extract was analyzed by high-performance liquid chromatography coupled to electrospray tandem mass spectrometry (LC-MS–MS). Chromatography was performed isocratically on Thermo Hypurity C₁₈ 5 μm analytical column, (50 mm × 4.6 mm i.d.). The assay of pegabalin was linear calibration curve over the range 10.000–10000.000 ng mL^?1. The lower limit of quantification was 10.000 ng mL^?1 in plasma. The method was successfully applied to the bioequivalence study of pregabalin capsules (150.0 mg) administered as a single oral dose.     

Protic acid (HClO4 supported on silica gel)-mediated synthesis of 2,3-unsaturated-O-glucosides and a chiral furan diol from 2,3-glycals

Perchloric acid supported on silica gel acts as an excellent reagent system in converting glucals into 2,3-unsaturated-O-glucosides in good to excellent yields in short reaction time with good alpha selectivity. Primary, secondary, and allylic alcohols, phenols, and thiols react with 3,4,6-tri-O-acetyl glucal with equal ease. In addition to this, a chiral furan diol is obtained from unprotected D-glucal or D-galactal in good yields.     

Army ants algorithm for rare event sampling of delocalized nonadiabatic transitions by trajectory surface hopping and the estimation of sampling errors by the bootstrap method

The most widely used algorithm for Monte Carlo sampling of electronic transitions in trajectory surface hopping (TSH) calculations is the so-called anteater algorithm, which is inefficient for sampling low-probability nonadiabatic events. We present a new sampling scheme (called the army ants algorithm) for carrying out TSH calculations that is applicable to systems with any strength of coupling. The army ants algorithm is a form of rare event sampling whose efficiency is controlled by an input parameter. By choosing a suitable value of the input parameter the army ants algorithm can be reduced to the anteater algorithm (which is efficient for strongly coupled cases), and by optimizing the parameter the army ants algorithm may be efficiently applied to systems with low-probability events. To demonstrate the efficiency of the army ants algorithm, we performed atom-diatom scattering calculations on a model system involving weakly coupled electronic states. Fully converged quantum mechanical calculations were performed, and the probabilities for nonadiabatic reaction and nonreactive deexcitation (quenching) were found to be on the order of 10(-8). For such low-probability events the anteater sampling scheme requires a large number of trajectories ( approximately 10(10)) to obtain good statistics and converged semiclassical results. In contrast by using the new army ants algorithm converged results were obtained by running 10(5) trajectories. Furthermore, the results were found to be in excellent agreement with the quantum mechanical results. Sampling errors were estimated using the bootstrap method, which is validated for use with the army ants algorithm.     

Enhancement of dielectric and electro-optical parameters of a newly prepared ferroelectric liquid crystal mixture by dispersing nano-sized copper oxide

ABSTRACT

Here, we present the effect of copper (II) oxide nanoparticles (nCuO) on dielectric and electro-optical parameters of a newly prepared ferroelectric liquid crystal (FLC) mixture, namely W302. The FLC mixture, comprising of pyrimidine compounds, was characterised through dielectric spectroscopy, differential scanning calorimetry (DSC), polarising optical microscopy (POM) and other electro-optical methods. The material parameters such as spontaneous polarisation, rotational viscosity, response time and tilt angle of W302 were found to be 14 nC/cm², 240 mPa.s, 150 µs and 28^?, respectively. The phase transition temperatures of W302 were observed through DSC and further confirmed by the dependence of dielectric loss factor in homogeneously aligned FLC sample with temperature. We also demonstrate the observance of a low-frequency dielectric relaxation mode due to the unwinding of the helix, called as partially unwound helical mode (p-UHM) along with Goldstone mode. The behaviour of p-UHM has been systematically studied with temperature and applied bias field. Further, dispersion of nCuO into host W302 has shown a significant increase in dielectric permittivity. Also, the p-UHM relaxation peak in the dielectric regime has disappeared with the incorporation of nCuO. These studies would be useful to fabricate better electro-optical devices for display, switching and beam steering applications. The formulation and characterization of a ferroelectric liquid crystal (FLC) mixture W302 composed of pyrimidine compounds is presented. Then, we observed the effect of copper (II) oxide nanoparticles (nCuO) on dielectric and electro-optical parameters of a newly prepared and characterized FLC mixture.     

Synthesis, Characterization and Antibacterial Activity of Some Transition Metal cis-3,7-dimethyl-2,6-octadiensemicarbazone Complexes

The synthesis and characterization of some transition metal cis-3,7-dimethyl-2,6-octadiensemicarbazone (CDOSC) complexes are reported. The ligand CDOSC yields: [ML₂ Cl₂] and [ML₂ Cl₂] Cl type complexes, where M = Cr^III, Mn^II, Fe^III, Co^II, Ni^II, Cu^II, Zn^II, Cd^II and Hg^II, L = CDOSC. Structures of the complexes were determined using elemental analysis, molar conductivity, magnetic measurements, i.r. and electronic, as well as n.m.r spectra. CDOSC acts as a bidentate ligand in all the complexes. All the newly synthesized metal complexes, as well as the ligand, were screened for their antibacterial activity. All the complexes exhibit strong inhibitory action against Gram (+) bacteria Staphylococcus aureus and Gram (−) bacteria Escherichia coli. The antibacterial activities of the complexes are stronger than those of the ligand CDOSC itself.     

High-Performance Thin-Layer Chromatographic Determination of Satranidazole in its Dosage Form

JPC – Journal of Planar Chromatography – Modern TLC - A high-performance thin-layer chromatographic method has been developed for determination of a new antiamoebic drug, satranidazole,...     

Thermal and biological studies of Schiff bases of chitosan derived from heteroaryl aldehydes

Journal of Thermal Analysis and Calorimetry - The synthesis of Schiff bases of chitosan is performed by the reaction of chitosan with different heteroaryl aldehydes, i.e., furfuraldehyde,...     

Synthesis,characterisation and ion exchange properties of hybrid organic–inorganic composite material: polyacrylamide zirconium (IV) iodosulphosalicylate

ABSTRACT

Contamination of groundwater by heavy metal is one of the most emerging and serious environmental problems. There are so many methods which are available to overcome these problems. Among various available methods, hybrid organic–inorganic ion exchange resin has become more popular due to certain advantages over other available conventional methods; hence, in the present proposed work, we synthesised a hybrid organic–inorganic composite material polyacrylamide zirconium (IV) iodosulphosalicylate by using the sol-gel technique. Synthesised resin was characterised by various methods like Infrared spectroscopy and Thermogravimetric analysis-Differential thermal analysis. Various samples of this ion exchange resin are prepared by changing the condition of synthesis, i.e. concentration of acrylamide to rationalise the ion exchange capacity of the synthesise hybrid organic–inorganic ion exchange resins. A mixture of 0.1 M potassium iodate, 0.1 M sulphosalicylic acid and 0.1 M acrylamide was added dropwise to 0.4 M zirconium oxychloride accompanied by constant stirring for 8 h using magnetic stirrer at 70°C to yield polyacrylamide zirconium (IV) iodosulphosalicylate with maximum ion exchange capacity. Ion exchange capacity of synthesised resin was determined by column method and the maximum ion exchange capacity was found for Pb(II). Determination of k_d values shows that the resin was highly selective for Pb (II).The selectivity for Pb was also evaluated by using certain binary mixture separation such as Ni (II)-Pb(II), Cu(II)-Pb(II), Cd(II)-Pb(II), Sr(II)-Pb(II), Ba(II)-Pb(II),Zn(II)-Pb(II) and Mg(II)-Pb(II).     

In vivo (31)P MRS study of skeletal muscle metabolism in patients with postpolio residual paralysis

The muscle metabolism of at-rest patients with varying degrees of postpolio residual paralysis (PPRP) was studied and compared with that of controls using in vivo phosphorus magnetic resonance spectroscopy. The phosphocreatine (PCr)/inorganic phosphate (Pi) and PCr/adenosine triphosphate ratios were lower in patients than in controls. Reduction in PCr/Pi suggests abnormalities in oxidative phosphorylation. A significant increase was observed in the phosphomonoester/PCr ratio in patients, indicating the accumulation of intermediary compounds of the glycolytic pathway. Furthermore, the phosphodiester/PCr ratio was also significantly increased in patients. In general, the observed changes in metabolite ratios were found to be related to the degree of residual paralysis, suggesting that metabolic changes are secondary to chronic neurogenic processes. These metabolic alterations appear to be the possible cause of energy deficit and underlying muscle fatigue in PPRP patients. The present results provide an insight into the metabolic impairment and degree of muscle damage in patients with PPRP.