Rapid determination of losartan and losartan acid in human plasma by multiplexed LC–MS/MS

A rapid LC–MS/MS method has been developed and validated for the determination of losartan (LOS) and its metabolite losartan acid (LA) (EXP‐3174) in human plasma using multiplexing technique (two HPLC units connected to one MS/MS). LOS and LA were extracted from human plasma by SPE technique using Oasis HLB® cartridge without evaporation and reconstitution steps. Hydroflumethiazide (HFTZ) was used as an internal standard (IS). The analytes were separated on Zorbax SB C‐18 column. The mass transition [M–H] ions used for detection were m/z 421.0 → 127.0 for LOS, m/z 435.0 → 157.0 for LA, and m/z 330.0 → 239.0 for HFTZ. The proposed method was validated over the concentration range of 2.5–2000 ng/mL for LOS and 5.0–3000 ng/mL for LA with correlation coefficient ?0.9993. The overall recoveries for LOS, LA, and IS were 96.53, 99.86, and 94.16%, respectively. Total MS run time was 2.0 min/sample. The validated method has been successfully used to analyze human plasma samples for applications in 100 mg fasted and fed pharmacokinetic studies.     

Acetalization of glycerol using mesoporous MoO3/SiO2 solid acid catalyst

Acetalization of glycerol with various aldehydes has been carried out using mesoporous MoO₃/SiO₂ as a solid acid catalyst. A series of MoO₃/SiO₂ catalysts with varying MoO₃ loadings (1–20 mol%) were prepared by sol–gel technique using ethyl silicate-40 and ammonium heptamolybdate as silica and molybdenum source respectively. The sol–gel derived samples were calcined at 500 °C and characterized using various physicochemical characterization techniques. The XRD of the calcined samples showed the formation of amorphous phase up to 10 mol% MoO₃ loading and at higher loading of crystalline α-MoO₃ on amorphous silica support. TEM analyses of the materials showed the uniform distribution of MoO₃ nanoparticles on amorphous silica support. Raman spectroscopy showed the formation of silicomolybdic acid at low Mo loading and a mixture of α-MoO₃ and polymolybdate species at high Mo loadings. Moreover the Raman spectra of intermediate loading samples also suggest the presence of β-MoO₃. Acetalization of glycerol with benzaldehyde was carried out using series of MoO₃/SiO₂ catalysts with varying MoO₃ loadings (1–20 mol%). Among the series, MoO₃/SiO₂ with 20 mol% MoO₃ loadings was found to be the most active catalyst in acetalization under mild conditions. Maximum conversion of benzaldehyde (72%) was obtained in 8 h at 100 °C with 60% selectivity for the six-membered acetal using 20% MoO₃/SiO₂. Interestingly with substituted benzaldehydes under same reaction conditions the conversion of aldehydes decreased with increase in selectivity for six-membered acetals. These results indicate the potential of this catalyst for the acetalization of glycerol for an environmentally benign process.     

Effect of anodic pH microenvironment on microbial fuel cell (MFC) performance in concurrence with aerated and ferricyanide catholytes

The performance of dual chambered microbial fuel cell (MFC, Nafion 117, non-catalyzed graphite electrodes) in concurrence with anodic pH microenvironment was evaluated based on bioelectricity generation and wastewater treatment efficiency. Experiments were carried out at different anodic pH microenvironments (acidophilic (6), neutral (7) and alkaline (8)) using both aerated and ferricyanide catholytes with mixed consortia as anodic biocatalyst employing chemical wastewater. Acidophilic pH in anodic chamber showed effective performance with respect to power output compared to the corresponding neutral and alkaline operations. However, substrate degradation was observed to be higher at neutral condition followed by alkaline and acidophilic operations. Ferricyanide as catholyte showed positive influence on the power output parameters compared to aerated catholyte. Nature of the catholyte did not show any visible influence on the wastewater treatment efficiency.     

A convergent approach towards the synthesis of the 2-alkyl-substituted tetrahydroquinoline alkaloid (−)-cuspareine

A convergent approach towards the synthesis of the 2-alkyl-substituted tetrahydroquinoline alkaloid (?)-cuspareine via enantiospecific construction of the (R)-benzyl 2-formyl-3,4-dihydroquinoline-1(2H)-carboxylate. We have achieved an efficient enantiospecific synthesis of (?)-cuspareine starting from known key starting materials. The reactions employed for individual transformations are simple and high yielding, and the strategy could potentially be easily extended.     

Mixed ionic and electronic conductivity study of charge transfer complexes of some substituted pyridines with iodine monochloride (ICl) by AC impedance spectroscopy

Mixed ionic and electronic conductivity of three solid charge transfer (CT) complexes of pyridine, 4-methylpyridine (γ-picoline) and 3,5-dimethylpyridine (3,5-lutidine) with ICl (iodine monochloride) are reported. Electrical parameters of the prepared complexes in the pellet form are evaluated at various temperatures and at wide frequency range by employing AC complex impedance spectroscopic technique. Suitable equivalent circuits for the Nyquist plots, which provide the most realistic model of the electrical properties of the CT complexes, have been suggested. Both transport number measurements and impedance spectra reveal that the conduction in γ-picoline-ICl complex is mainly due to ions, in 3,5-dimethylpyridine-ICl complex, it is due to both ions and electrons and in pyridine-ICl complex, it is predominantly due to electrons. The a.c. conductivity measurements of the CT complexes have been carried out in the frequency range of 10–10⁵ Hz within the temperature range of 303–353 K. The variation of a.c. conductivity with frequency follows the Jonscher’s universal power law. The temperature dependence of electrical conductivity suggests the semiconducting behaviour of the materials.     

Relation Between CPT Violation in Neutrino Masses and Mixings

The neutrino parameters determined from the solar neutrino data and the anti-neutrino parameters determined from KamLAND reactor experiment are in good agreement with each other. However, the best fit points of the two sets differ from each other by about 10⁻⁵ eV² in mass-square difference and by about 2° in the mixing angle. Future solar neutrino and reactor anti-neutrino experiments are likely to reduce the uncertainties in these measurements. This, in turn, can lead to a signal for CPT violation in terms a non-zero difference between neutrino and anti-neutrino parameters. In this paper, we propose a CPT violating mass matrix which can give rise to the above differences in both mass-squared difference and mixing angle and study the constraints imposed by the data on the parameters of the mass matrix.     

Conformationally rigid chiral ferrocene derivative: Synthesis,resolution and stereochemical assignment

A conformationally rigid chiral molecule LB-I with Lewis basic site has been designed and synthesized in racemic form from ferrocene via Lewis acid mediated diastereoselective cyclization of hydroxy lactam. Both isomers were successfully obtained in enantiomerically pure form through classical resolution using dibenzoyl-d-tartaric acid as the chiral resolving agent in acetone. The nature of the diastereomeric salt formed in the resolution process was investigated by single crystal X-ray crystallographic studies. The absolute configuration of (+)-LB-I was unambiguously assigned as (S,R_p) by single crystal analysis of the salt I obtained from precipitate fraction containing (+)-LB-I and dibenzoyl-d-tartaric acid.     

Synthesis of 2-amino-3-cyano-4H-chromen-4-ylphosphonates and 2-amino-4H-chromenes catalyzed by tetramethylguanidine

Synthesis of 2-amino-4H-chromen-4-ylphosphonates and 2-amino-4H-chromenes has been accomplished by the reaction of salicylaldehyde, malononitrile, dialkyl/diphenylphosphites catalyzed by 1,1,3,3-tetramethylguanidine (TMG) under neat conditions at room temperature. The applicability of catalytic TMG for the synthesis of 2-amino-4H-chromenes also has been described. The mild reaction conditions, simple work-up procedure, and use of TMG as an inexpensive catalyst provides an economical protocol for the preparation of important phosphorus-containing compounds.     

Effect of substrate bias voltage on the structure, electric and dielectric properties of TiO2 thin films by DC magnetron sputtering

Titanium dioxide (TiO₂) films have been deposited on glass and p-silicon (1 0 0) substrates by DC magnetron sputtering technique to investigate their structural, electrical and optical properties. The surface composition of the TiO₂ films has been analyzed by X-ray photoelectron spectroscopy. The TiO₂ films formed on unbiased substrates were amorphous. Application of negative bias voltage to the substrate transformed the amorphous TiO₂ into polycrystalline as confirmed by Raman spectroscopic studies. Thin film capacitors with configuration of Al/TiO₂/p-Si have been fabricated. The leakage current density of unbiased films was 1 × 10⁻⁶ A/cm² at a gate bias voltage of 1.5 V and it was decreased to 1.41 × 10⁻⁷ A/cm² with the increase of substrate bias voltage to −150 V owing to the increase in thickness of interfacial layer of SiO₂. Dielectric properties and AC electrical conductivity of the films were studied at various frequencies for unbiased and biased at −150 V. The capacitance at 1 MHz for unbiased films was 2.42 × 10⁻¹⁰ F and it increased to 5.8 × 10⁻¹⁰ F in the films formed at substrate bias voltage of −150 V. Dielectric constant of TiO₂ films were calculated from capacitance–voltage measurements at 1 MHz frequency. The dielectric constant of unbiased films was 6.2 while those formed at −150 V it increased to 19. The optical band gap of the films decreased from 3.50 to 3.42 eV with the increase of substrate bias voltage from 0 to −150 V.