A Validated LC Method for Separation and Quantification of Voriconazole and Its Enantiomer

A simple liquid chromatographic method was developed for the separation and quantification of voriconazole and its enantiomer in drug substance. The separation was achieved on Chiral cel-OD (250 mm × 4.6 mm × 10 μm) using mobile phase consisting of n-hexane and ethanol in the ratio 9:1 (v/v) with a flow rate of 1.0 mL min⁻¹, at 27 °C column temperature and detection at 254 nm with an injection volume of 20 μL. Ethanol was used as diluent. The method is capable of detecting the (2S, 3R) enantiomer down to 0.0075% and can quantify down to 0.021% with respect to sample concentration. The method is rapid and the resolution achieved was about 3.0. This method can be employed for the quantification of (2S, 3R) enantiomer in voriconazole drug substance.     

Strategies for controlling the active layer morphologies in OPVs

This review focuses on the recent developments in our understanding of active layer morphologies for organic photovoltaic cells and approaches to obtain active layer morphologies for high power conversion efficiencies. The evolution of active layer morphologies, as studied by high resolution electron microscopy, X-ray and neutron scattering, and dynamic secondary ion mass spectrometry, is covered, along with strategies including the use of small molecule additives, polymer nanowires and polymer nanoparticles to realize active layer morphologies. © 2012 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2012     

Rational selection of structurally diverse natural product scaffolds with favorable ADME properties for drug discovery

Natural product analogs are significant sources for therapeutic agents. To capitalize efficiently on the effective features of naturally occurring substances, a natural product-based library production platform has been devised at Aurigene for drug lead discovery. This approach combines the attractive biological and physicochemical properties of natural product scaffolds, provided by eons of natural selection, with the chemical diversity available from parallel synthetic methods. Virtual property analysis, using computational methods described here, guides the selection of a set of natural product scaffolds that are both structurally diverse and likely to have favorable pharmacokinetic properties. The experimental characterization of several in vitro ADME properties of twenty of these scaffolds, and of a small set of designed congeners based upon one scaffold, is also described. These data confirm that most of the scaffolds and the designed library members have properties favorable to their utilization for creating libraries of lead-like molecules.These authors have contributed equally to this work.     

Modified thermal balance method for estimating minimum inerting concentraion of flammable refrigerant mixtures

R1234yf is considered as a better alternative for R134a (the conventional refrigerant) due to its low global warming potential value, while its usage is limited because of its flammability. The flammability of any flammable refrigerant can be reduced by adding dilutants that are inert. Two methods (group contribution method and thermal balance method) were used to estimate the minimum inerting concentration (which decides the flammability zone) of the binary mixtures (refrigerant?+?dilutant). It was observed that the group contribution method and the thermal balance method predicted minimum inerting concentration of the refrigerant mixture (refrigerant?+?dilutant) with an absolute error of more than 50% and 8%, respectively. Therefore, a modified thermal balance method is proposed in this study to estimate the minimum inerting concentration and found that the proposed method predicts the values with reasonable accuracy when compared with the available experimental data. Further, the minimum inerting concentration for the dilutants R125 and R245fa (that are not experimentally known) with R1234yf is estimated. The results indicated that R227ea has better inert effect with R1234yf when compared to other dilutants (R125, R134a and R245fa) considered in this study. It was also found that the critical inerting concentration for R1234yf is 36.5%.

     

Spectroscopic investigations on PbO–As2O3 glasses crystallized with TiO2

PbO–As₂O₃ glasses mixed with different concentrations of TiO₂ (ranging from 0 to 1.0 mol%) were crystallized. The samples were characterized by X-ray diffraction, scanning electron microscopy and energy dispersive spectroscopy (EDS) techniques. Studies were extended to optical absorption, IR, ESR, luminescence and magnetic susceptibility on these samples. The X-ray diffraction studies reveal the presence of Pb₃O₄, Ti(As₂O₇), Pb(As₂O₆), Pb₃(AsO₄)₂ PbTi₃O₇ and Ti₂O₃ crystal phases. The optical absorption studies together with ESR and magnetic susceptibility measurements indicated that the titanium ions exist in both Ti³⁺ and Ti⁴⁺ states in all the samples and there is an increase in titanium ions in the trivalent state with increasing concentration of nucleating agent TiO₂. The quantitative analysis of these results indicated that there is a growing degree of disorder in the glass network with increasing concentration of the crystallizing agent. The luminescence studies indicated that the samples crystallized with low concentrations of TiO₂ show high luminescence efficiency in the visible region.     

Apical functionalization of chiral heterohelicenes

We describe a synthetic protocol to selectively functionalize chiral bridged triarylamines at the apical position using regioselective copper-catalyzed amination reaction. This protocol allows the coupling of diphenylamines with a sterically hindered but electronically activated aryl-Br bond in the presence of a sterically unhindered but electronically unactivated aryl-Br bond. The unactivated aryl-Br bond was utilized further to synthesize a chiral heterohelicene homodimer using Stille coupling.     

Ag concentration dependent transport properties of LiF-MoO3-P2O5 glasses

LiF-MoO₃-P₂O₅ glasses mixed with different concentrations of Ag₂O (ranging from 0 to 1.0 mol%) was prepared. D.C. conductivity and dielectric properties over a range of temperature have been investigated. The analysis of the results of d.c. conductivity has indicated that T>θ_D/2, the small polaron hoping model seems to be fit and the conduction is adiabatic in nature. These results further indicated that there is a change over of conduction mechanism from electronic to ionic at about 0.4 mol% of Ag₂O. The low temperature part of a.c. conductivity is explained based on quantum mechanical tunneling model. The quantitative analysis of these results is further extended with the aid of the data on optical absorption, ESR and IR spectral studies.     

ESI‐MS/MS analysis of protonated N‐methyl amino acids and their immonium ions

Methylation is one of the important posttranslational modifications of biological systems. At the metabolite level, the methylation process is expected to convert bioactive compounds such as amino acids, fatty acids, lipids, sugars, and other organic acids into their methylated forms. A few of the methylated amino acids are identified and have been proved as potential biomarkers for several metabolic disorders by using mass spectrometry–based metabolomics workstation. As it is possible to encounter all the N‐methyl forms of the proteinogenic amino acids in plant/biological systems, it is essential to have analytical data of all N‐methyl amino acids for their detection and identification. In earlier studies, we have reported the ESI‐MS/MS data of all methylated proteinogenic amino acids, except that of mono‐N‐methyl amino acids. In this study, the N‐methyl amino acids of all the amino acids ( 1 ‐ 21 ; including one isomeric pair) were synthesized and characterized by ESI‐MS/MS, LC/MS/MS, and HRMS. These data could be useful for detection and identification of N‐methyl amino acids in biological systems for future metabolomics studies. The MS/MS spectra of [M + H]⁺ ions of most N‐methyl amino acids showed respective immonium ions by the loss of (H₂O, CO). The other most common product ions detected were [MH‐(NH₂CH₃]⁺, [MH‐(RH)]⁺ (where R = side chain group) ions, and the selective structure indicative product ions due to side chain and N‐methyl group. The isomeric/isobaric N‐methyl amino acids could easily be differentiated by their distinct MS/MS spectra. Further, the MS/MS of immonium ions inferred side chain structure and methyl group on α‐nitrogen of the N‐methyl amino acids.     

An Organic Dyad Composed of Diathiafulvalene‐Functionalized Diketopyrrolopyrrole–Fullerene for Single‐Component High‐Efficiency Organic Solar Cells

A new low‐band gap dyad DPP‐Ful, which consists of covalently linked dithiafulvalene‐functionalized diketopyrrolopyrrole as donor and fullerene (C₆₀) as the acceptor, has been designed and synthesized. Organic solar cells were successfully constructed using the DPP‐Ful dyad as an active layer. This system has a record power‐conversion efficiency (PCE) of 2.2 %, which is the highest value when compared to reported single‐component organic solar cells.