Analysis of duloxetine hydrochloride and its related compounds in pharmaceutical dosage forms and in vitro dissolution studies by stability indicating UPLC

A reproducible gradient reversed-phase ultra-performance liquid chromatographic method is developed for quantitative determination of duloxetine hydrochloride in pharmaceutical dosage forms. The method is also applicable for analysis of related substances and for study of in vitro dissolution profiles. Chromatographic separation is achieved on a 50 mm × 4.6 mm, 1.8 μm C-18 column. Mobile phase A contains a mixture of 0.01 M KH(2)PO(4) (pH 4.0) buffer, tetrahydro furan, and methanol in the ratio 67:23:10 (v/v/v), respectively, and mobile phase B contains a mixture of 0.01 M KH(2)PO(4), (pH 4.0) buffer, and acetonitrile in the ratio 60:40 (v/v), respectively. The flow rate is 0.6 mL/min, and the detection wavelength is monitored at 236 nm. Resolution of duloxetine hydrochloride and three potential impurities is greater than 2.0 for all pairs of components. The drug was subjected to ICH prescribed hydrolytic, oxidative, photolytic, and thermal stress conditions. Method is validated for linearity, specificity, accuracy, precision, ruggedness, and robustness.     

O‐Alkylation of Pyridine Aldo‐ and Ketoximes with Dihalohydrins under Phase‐Transfer Conditions

Phase‐transfer‐catalyzed alkylation of (E)‐pyridine aldo‐ and (E)‐ketoximes with dihalohydrins in the benzene (or DMSO)/10% aq. NaOH system in the presence of tetradecylammonium bromide proceeds regiospecifically to afford the corresponding O‐halohydrins in good yields. In this study, first O‐halohydrin derivatives were converted into glycidyl ether derivatives, and then a new series of amino alcohols were synthesized by the condensation of amines with these glycidyl ethers.     

Synthetic Access to New Carbamate and Thiocarbamate Derivatives from Pyridinecarbaldehyde Oximes and Hydroxypyridines

The synthesis of pyridine carbamate and thiocarbamate derivates is described. A series of oxime carbamate and thiocarbamate derivatives were synthesized by the addition of 2-, 3-, and 4-pyridinecarbaldehyde oximes to isocyanates and isothiocyanates. Furthermore, carbamate and thiocarbamate derivatives of pyridine were synthesized by the addition of 2-, 3-, and 4-hydroxy pyridine to isocyanates and isothiocyanates. Their structures were confirmed by both analytical and spectral data.

Synthesis of a novel calix[4]azacrown ionophore and its extraction ability toward Cr(VI)

The present study describes the synthesis of a novel extractant p-tert-butyl-calix[4]azacrown ionophore (5) and evaluation of its extraction capability toward dichromate ion from aqueous solution. At first, p-tert-butyl-calix[4]azacrown ionophore (5) has been synthesized from the condensation of p-tert-butyl-calix[4]arene diamine (3) with N-(4-formylphenyl)-aza-15-crown-5 (4). The studies regarding the removal of dichromate ion from the aqueous solutions have been carried out in the liquid–liquid extraction systems. The extraction results showed that p-tert-butyl-calix[4]azacrown derivative (5) exhibited generally higher affinity towards dichromate ion than both 3 and 4 at all studied pHs.     

Light-scattering experiments in dye-doped liquid crystals both to determine crystal parameters and to construct consistent neural network empirical physical formulas for scattering amplitudes

The aim of this paper is two-fold. Firstly, static laser light-scattering amplitude measurements in azo-dye doped nematic liquid crystals (NLCs) were made versus scattering angle, temperature and applied bias voltage. Three NLC parameters were determined: the elastic constant ratios K₁₁/K₂₂ by regression, phase transition temperatures, and Freedericksz voltages from the graphs. They were all doping ratio dependent. Secondly, as a novel approach, by a nonlinear universal function approximator layered feedforward neural network (LFNN) we constructed an explicit form of empirical physical formulas (EPFs) for theoretically unknown nonlinear azo-dye doped NLC scattering amplitude functions. Excellent LFNN test set (i.e. yet-to-be measured experimental data) predictions prove that the constructed LFNN-EPPs estimate unknown amplitude functions consistently. The LFFN-EPFs, too, confirmed the doping-ratio dependency. Also, comparing LFNN and regression amplitude fits, the LFNN fits were significantly better. In conclusion, physical laws embedded in the physical data can be consistently extracted by LFNN. One major potential application in the nonlinear optics domain is that these LFNN-EPFs, by differentiation, integration, minimization, etc., can be used to obtain further NLC scattering amplitude related molecular structural physical quantities. This could in turn help us to develop new nonlinear optical materials.     

A novel method degrading the combined effect of FWM and ASE noise in WDM systems containing in-line optical amplifiers

In this paper, a novel method degrading the combined effect of four-wave mixing (FWM) and amplified spontaneous emission (ASE) noise of the amplifier on the most heavily affected channel in an equally channel spaced wavelength division multiplexing (WDM) system containing in-line optical amplifiers is proposed. FWM effect is directly related to input powers of channels. So, FWM effect can be degraded by controlling channel input powers. In the proposed method, varying the input power of each channel in an optical fiber, the output optical signal to noise ratio (OSNR) values are evaluated and input powers of all channels are optimized in order to maximize the OSNR value of the channel having the lowest OSNR. To interpret the results obtained, output OSNR values for the minimum optical input power launched to the system by each channel are also computed. Being compared to the computed results for minimum optical input powers, the lowest output OSNR value among all channels for optimized input powers shows a 5.1867 dB increase in a 5-channel system, a 3.5988 dB increase in a 9-channel system, a 3.0855 dB increase in a 15-channel system and a 1.6795 dB increase for a 21-channel system. Furthermore, output OSNR values of all channels exhibit a significant increase.     

Influence of molecular weight on the short‐channel effect in polymer‐based field‐effect transistors

In this study, we demonstrate how the intrinsic properties of a polymer can influence the electrical characteristics of organic field‐effect transistors (OFETs). OFETs fabricated with three batches of poly[2‐methoxy,5‐(3′,7′‐dimethyl‐octyloxy)]‐p‐phenylene vinylene (MDMO‐PPV) were investigated. The properties of the polymers were initially investigated using Fourier transform infrared spectroscopy (FTIR), impedance spectroscopy (IS), gel permeation chromotography (GPC), and cyclic voltammetry (CV), respectively. The structure and purity of the polymer batches were found to be very comparable, but the molecular weight (M_n and M_w) and polydispersity (PDI = M_w/M_n), varied between the samples and the HOMO and LUMO levels of the polymers were found to depend on the molecular weight properties. OFETs were then fabricated with the polymers and electrically characterized. It was observed that the channel current and the field‐effect mobility increase with increasing polymer molecular weight. The output characteristics of the transistors, on the other hand, were found to depend on the PDI of the polymer. Saturation of the channel current occurs at higher source–drain voltages and short‐channel behavior was observed to start at longer channel lengths for polymers with a higher PDI. This behavior is observed to be thickness dependent, and the short‐channel behavior was more pronounced for thicker MDMO‐PPV films. These results are explained in terms of influences of chain packing and ordering and high bulk currents on the FET output and transistor parameters. © 2011 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 50: 117–124, 2012     

High-resolution 13C NMR study of free and metal-complexed ionophores in the solid state: Conformation and dynamics of the macrocyclic ring and the effect of intermolecular short contact of methyl groups on spin–lattice relaxation times and displacements of chemical shifts

High-resolution ¹³C NMR spectra of 15 samples of uncomplexed and metal-complexed tetranactin and nonactin were recorded in the solid state, revealing characteristic displacements of peaks due to complex formation and the effect of crystalline packing on the ¹³C chemical shifts and spin–lattice relaxation times of the methyl groups. The C-1 ¹³C chemical shifts of uncomplexed and complexed tetranaction and nonactin are well related to the variation of nearby torsion angles characteristic of the macrocyclic conformation, as determined by x-ray diffraction. The existence of short intermolecular contact of methyl groups (<3.8 Å) at the surface of the molecules results in either prolonged ¹³C spin–lattice relaxation times in the laboratory frame (T₁^C) or substantial upfield displacement of peaks (up to 6 ppm). In addition, significantly reduced T₁^C values in uncomplexed nonactin (one order of magnitude smaller than those of other compounds) was ascribed to the presence of a puckering motion of the tetrahydrofuran ring and fluctuation of the macrocyclic ring in the solid state (with a time scale of 10⁻⁸ _s). Finally, how the conformations of these compounds in the solid are retained in chloroform solution was examined in view of the differences in the ¹³C chemical shifts between the solid and solution.