Compatibility studies between nebicapone,a novel COMT inhibitor,and excipients using stepwise isothermal high sensitivity DSC method

Study of excipients incompatibility with drugs in an early phase of pharmaceutical development is still a persistent difficulty within the pharmaceutical industry. We examine here the compatibility between an experimental drug (nebicapone) and common excipients using differential scanning calorimetry (DSC), high sensitivity DSC (HSDSC) and a conventional heat stress test. The results obtained indicate that nebicapone may be compatible with lactose monohydrate and sodium croscarmellose but is incompatible with magnesium stearate. This study concludes that HSDSC, in stepwise isothermal mode, may be used as a potential tool for detecting excipient incompatibilities.     

Study of the Light‐Induced Spin Crossover Process of the [FeII(bpy)3]2+ Complex

Ab initio calculations have been performed on [Fe^II(bpy)₃]²⁺ (bpy=bipyridine) to establish the variation of the energy of the electronic states relevant to light‐induced excited‐state spin trapping as a function of the Fe? ligand distance. Light‐induced spin crossover takes place after excitation into the singlet metal‐to‐ligand charge‐transfer (MLCT) band. We found that the corresponding electronic states have their energy minimum in the same region as the low‐spin (LS) state and that the energy dependence of the triplet MLCT states are nearly identical to the ¹MLCT states. The high‐spin (HS) state is found to cross the MLCT band near the equilibrium geometry of the MLCT states. These findings give additional support to the hypothesis of a fast singlet–triplet interconversion in the MLCT manifold, followed by a ³MLCT–HS (⁵T₂) conversion accompanied by an elongation of the Fe? N distance.     

Free-standing urethane/urea elastomer films undoped and doped with ferro-nano-particles

We report on an experimental study of the structures presented by urethane/urea elastomeric films without and with ferromagnetic nanoparticles incorporated. The study is made by using the X-ray diffraction, nuclear magnetic resonance (NMR), optical, atomic and magnetic force (MFM) microscopy techniques, and mechanical assays. The structure of the elastomeric matrix is characterized by a distance of 0.46nm between neighboring molecular segments, almost independent on the stretching applied. The shear casting performed in order to obtain the elastomeric films tends to orient the molecules parallel to the flow direction thus introducing anisotropy in the molecular network which is reflected on the values obtained for the orientational order parameter and its increase for the stretched films. In the case of nanoparticles-doped samples, the structure remains nearly unchanged although the local order parameter is clearly larger for the undoped films. NMR experiments evidence modifications in the molecular network local ordering. Micrometer size clusters were observed by MFM for even small concentration of magnetic particles.     

EELS characterization of radiolytic products in frozen samples

Electron energy loss spectroscopy (EELS) was used to obtain information about the radiation chemistry of frozen aqueous specimens in the electron microscope by observing the hydrogen and oxygen K-edges. Measurements on frozen solutions of 30% hydrogen peroxide revealed the presence of molecular oxygen identified by a distinct 531-eV peak at the O K-edge even for electron doses below 100 e/nm2. The molecular oxygen content of irradiated H?O? solution was determined by least squares fitting of O K-edge reference spectra from water and gas-phase oxygen. It was found that the fraction of molecular oxygen to water oxygen was in the range 0.03-0.05. EELS from pure frozen water showed no features attributable to molecular oxygen or molecular hydrogen (K edge at ~13 eV) even at high electron doses above 10? e/nm2. Spectra from frozen sucrose and protein solutions and their mixtures, however, did show evolution of a molecular hydrogen peak at ~13 eV for doses above 10? e/nm2, consistent with previous measurements and indicative of hydrogen bubble formation. Molecular oxygen was not observed in any of the frozen solutions of organic compounds indicating that oxygen is not a major product of free radical decay, in contrast to molecular hydrogen formation.     

Processing discontinuous displacement fields by a spatio-temporal derivative technique

In this paper, a digital image correlation (DIC) method coupling cross-correlation with spatio-temporal differential techniques was proposed for assessing discontinuous displacement fields. The accuracy and robustness of the algorithm was assessed on a set of numerical tests by processing computer generated speckled-pattern images. Fracture mechanical tests in mode I were considered, in which both in-plane and out-of-plane rigid-body movements were taken into account. The ability for recovering the analytical asymptotic displacement field in mode I was analysed, and stress intensity factor, crack opening displacement and crack tip location were used as quantitative parameters for validation purposes. Throughout these tests, the results obtained with the proposed method were systematically compared to the ones from Aramis DIC-2D commercial code. Globally, the results computed from both methods are in good agreement with reference values. However, due to the high spatial resolution (point-wise characteristic), a better matching of the displacements in the neighbour of discontinuities could be obtained by the proposed method.     

Combination of Raman, Infrared, and X-Ray Energy-Dispersion Spectroscopies and X-Ray Diffraction to Study a Fossilization Process

X-ray diffraction was combined with X-ray energy-dispersion, Fourier-transform infrared, and Raman spectroscopies to study the fossilization of a Cretaceous specimen of the plant Brachyphyllum castilhoi, a fossil from the Ipubi Formation, in the Araripe Sedimentary Basin, Northeastern Brazil. Among the possible fossilization processes, which could involve pyrite, silicon oxide, calcium oxide, or other minerals, we were able to single out pyritization as the central mechanism producing the fossil, more than 100 million years ago. In addition to expanding the knowledge of the Ipubi Formation, this study shows that, when combined with other experimental techniques, Raman spectroscopy is a valuable tool at the paleontologist’s disposal.     

Selecting green suppliers based on GSCM practices: Using fuzzy TOPSIS applied to a Brazilian electronics company

Due to an increased awareness and significant environmental pressures from various stakeholders, companies have begun to realize the significance of incorporating green practices into their daily activities. This paper proposes a framework using Fuzzy TOPSIS to select green suppliers for a Brazilian electronics company; our framework is built on the criteria of green supply chain management (GSCM) practices. An empirical analysis is made, and the data are collected from a set of 12 available suppliers. We use a fuzzy TOPSIS approach to rank the suppliers, and the results of the proposed framework are compared with the ranks obtained by both the geometric mean and the graded mean methods of fuzzy TOPSIS methodology. Then a Spearman rank correlation coefficient is used to find the statistical difference between the ranks obtained by the three methods. Finally, a sensitivity analysis has been performed to examine the influence of the preferences given by the decision makers for the chosen GSCM practices on the selection of green suppliers. Results indicate that the four dominant criteria are Commitment of senior management to GSCM; Product designs that reduce, reuse, recycle, or reclaim materials, components, or energy; Compliance with legal environmental requirements and auditing programs; and Product designs that avoid or reduce toxic or hazardous material use.     

Assessing the antioxidative properties and chemical composition of Linaria vulgaris infusion

The ability of Linaria vulgaris (Scrophulariaceae) infusion to act as a scavenger of 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical, reactive oxygen species (superoxide radical, hydroxyl radical, hypochlorous acid (HOCl)) and nitric oxide was investigated. The obtained data indicate that the infusion has a good scavenging activity against superoxide radical and is a very potent nitric oxide and DPPH scavenger. In hydroxyl radical assay a pro-oxidant capacity was noticed, especially for concentrations higher than 31.25 microg mL(-1). No effect was found against HOCl. A phytochemical study of this extract was also performed. The HPLC/UV analysis allowed the identification and quantification of eight organic acids (oxalic, aconitic, citric, ketoglutaric, ascorbic, malic, shikimic and fumaric acids). The phenolic composition of the lyophilised infusion was also determined by HPLC/DAD and four compounds were quantified, but, despite its high content, only linarin was managed to be identified.