Capillary electrophoresis method for the determination of isradipine enantiomers: stability studies and pharmaceutical formulation analysis

A simple enantioselective method based on CE using CD as chiral selector was developed and validated for the determination of isradipine (IRD) enantiomers in a pharmaceutical formulation and for the determination of IRD enantiomers in degradation studies. After optimization, the best results were obtained using 15 mM borate buffer at pH 9.3 and sulfobutyl ether-β-cyclodextrin (2.5%, w/v) as chiral selector. The applied voltage was +30 kV, and the sample injection was performed in the hydrodynamic mode. All analyses were carried out in a fused-silica uncoated capillary with an id of 50 μm and total length of 60.0 cm. Under these conditions, a complete separation between IRD enantiomers was achieved in less than 7 min. Linearity was obtained in the range 50-300 μg/mL for both enantiomers (r≥0.9978). The RSD (%) and relative errors (%) obtained in precision and accuracy studies (intra-day and inter-day) were lower than 5%. Therefore, this method was found to be appropriate for controlling pharmaceutical formulations containing IRD enantiomers and the assay was considered to be stability indicating. The drug was subjected to oxidation, hydrolysis and photolysis. In all stress conditions the drug presented considerable degradation when compared with a fresh sample (zero time).     

Magnetic and transport properties of transition-metal implanted ZnO single crystals

ZnO single crystals were implanted with Mn, Co and Ni with fluences between 1 × 10¹⁶ cm^-2 and 1 × 10¹⁷ cm^-2 and energy of 200 keV. Results indicate that aggregation of transition metal ions in the as implanted state occurs only in the case of Ni. After an annealing stage to recover the ZnO structure aggregation occurs for the higher fluences of all implanted species. For lower concentrations paramagnetic behaviour with magnetic moments close to those of individual ions is observed. No polarised impurity band is formed as a result of the presence of transition metal ions and all samples show electrical conduction by carriers in extended states of ZnO. Significant values of magnetoresistance are measured at low temperatures, where electrical transport is described by hopping mechanisms between localized states. The sign of the magnetoresistance is dependent of the doping ion and is correlated with the observed aggregation.     

An improved weighted essentially non-oscillatory scheme for hyperbolic conservation laws

In this article we develop an improved version of the classical fifth-order weighted essentially non-oscillatory finite difference scheme of [G.S. Jiang, C.W. Shu, Efficient implementation of weighted ENO schemes, J. Comput. Phys. 126 (1996) 202–228] (WENO-JS) for hyperbolic conservation laws. Through the novel use of a linear combination of the low order smoothness indicators already present in the framework of WENO-JS, a new smoothness indicator of higher order is devised and new non-oscillatory weights are built, providing a new WENO scheme (WENO-Z) with less dissipation and higher resolution than the classical WENO. This new scheme generates solutions that are sharp as the ones of the mapped WENO scheme (WENO-M) of Henrick et al. [A.K. Henrick, T.D. Aslam, J.M. Powers, Mapped weighted essentially non-oscillatory schemes: achieving optimal order near critical points, J. Comput. Phys. 207 (2005) 542–567], however with a 25% reduction in CPU costs, since no mapping is necessary. We also provide a detailed analysis of the convergence of the WENO-Z scheme at critical points of smooth solutions and show that the solution enhancements of WENO-Z and WENO-M at problems with shocks comes from their ability to assign substantially larger weights to discontinuous stencils than the WENO-JS scheme, not from their superior order of convergence at critical points. Numerical solutions of the linear advection of discontinuous functions and nonlinear hyperbolic conservation laws as the one dimensional Euler equations with Riemann initial value problems, the Mach 3 shock–density wave interaction and the blastwave problems are compared with the ones generated by the WENO-JS and WENO-M schemes. The good performance of the WENO-Z scheme is also demonstrated in the simulation of two dimensional problems as the shock–vortex interaction and a Mach 4.46 Richtmyer–Meshkov Instability (RMI) modeled via the two dimensional Euler equations.     

In vitro photodynamic antimicrobial chemotherapy in dentine contaminated by cariogenic bacteria

The development of a method to ensure bacterial-free substrates without extensive cavity preparation would be highly useful to dentistry, since there is no currently available effective method for killing residual bacteria in dentinal tissue. This randomized in vitro study determined parameters for using toluidine blue O (TBO) with a light-emitting diode (LED) for dentine caries disinfection and monitored intrapulpal/periodontal temperatures during irradiation. Occlusal human dentine slabs were immersed in Streptococcus mutans culture for demineralization induction. Slabs were allocated to 10 groups (n = 15), which were treated with 0.1 mg ml⁻¹ TBO with 5 min of incubation time or 0.9% NaCl solution for 5, 10 or 15 min, and submitted or not to irradiation for 5, 10 or 15 min (47, 94, and 144 J/cm²). Before and after treatments, dentine samples were analyzed with regard to S. mutans counts. In whole teeth, temperature in pulp and periodontium was measured by thermocouples during irradiation. Kruskal-Wallis/Student-Newman-Keuls, and ANOVA/Tukey test were respectively utilized to compare log reductions and temperature rises between groups. Bacterial reduction was observed when dentine was exposed to both TBO and LED at all irradiation times, as well as to LED alone for 10 and 15 min. Temperature increases lower than 2°C were observed for either pulp or periodontium. Concluding, LED combined with TBO is a safe and effective approach for dentine caries disinfection. Nevertheless, additional studies should be conducted to determine the influence of the irradiation in S. mutans viability in dentinal surface/tubules.     

Neuropeptide delivery to the brain: a von Willebrand factor signal peptide to direct neuropeptide secretion

Background  

Multiple neuropeptides, sometimes with opposing functions, can be produced from one precursor gene. To study the roles of the different neuropeptides encoded by one large precursor we developed a method to overexpress minigenes and establish local secretion.     

Alternative Extraction and Downstream Purification Processes for Anthocyanins

Anthocyanins are natural pigments displaying different attractive colors ranging from red, violet, to blue. These pigments present health benefits that increased their use in food, nutraceuticals, and the cosmetic industry. However, anthocyanins are mainly extracted through conventional methods that are time-consuming and involve the use of organic solvents. Moreover, the chemical diversity of the obtained complex extracts make the downstream purification step challenging. Therefore, the growing demand of these high-value pigments has stimulated the interest in designing new, safe, cost-effective, and tunable strategies for their extraction and purification. The current review focuses on the potential application of compressed fluid-based (such as subcritical and supercritical fluid extraction and pressurized liquid extraction) and deep eutectic solvents-based extraction methods for the recovery of anthocyanins. In addition, an updated review of the application of counter-current chromatography for anthocyanins purification is provided as a faster and cost-effective alternative to preparative-scale HPLC.     

Effect of Non-Calcined Sugarcane Bagasse Ash as an Alternative Precursor on the Properties of Alkali-Activated Pastes

BFS-MK-based alkali-activated materials are well established as an alternative for sustainable and green construction. This work aims to collaborate and encourage the use of biomass ashes, such as sugarcane bagasse ash (SCBA), as a precursor in alkali-activated materials (AAM). This ash is a rich source of aluminosilicate, which is a primary requirement for this application. In addition, this waste is still an environmental liability, especially in developing countries, and with a large volume of annual production. Thus, in this research, alkali-activated pastes (AA) were produced using sugarcane bagasse ash (SCBA), granulated blast furnace slag (BFS) and metakaolin (MK) as precursors. In addition, environmental gains were encouraged with energy savings, with no extra reburn or calcination steps in the SCBA. Thus, the precursors were characterized by laser granulometry, X-ray fluorescence spectrometry (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). The pastes were produced by mixing the precursors with the activator, composed of a mixture of sodium hydroxide 8 mol/L and sodium silicate. Aiming to study the incorporation of SCBA, all samples have a precursor/activator ratio and a BFS/(BFS + MK) ratio constant of 0.6. The compressive strength analysis, FTIR, XRD, TGA, SEM and isothermal calorimetry analyses pointed out the occurrence of alkaline activation in all proposed samples for curing times of 7, 28 and 91 days. The sample GM0.6-BA0 (15% SCBA) achieved the highest compressive strength among the samples proposed (117.7 MPa, at 91 days), along with a good development of strength throughout the curing days. Thus, this work presents the properties of alkaline-activated pastes using SCBA as a sustainable and alternative precursor, seeking to encourage the use of raw materials and alternative waste in civil construction.