Reverse Phase HPLC Methodology for the Determination of Bay K8644.

Following ICH guidelines for analytical validation, we report a common C18 column stability indicating isocratic reverse phase high performance liquid chromatography method for the determination of the ion channel modulator Bay K8644. Two main forced degradation products and a minor impurity were also tentatively identified by Mass Spectrometry. The mobile phase consisted of a 50/50 acetonitrile/buffer mixture at a flow rate of 2 mL/min. Mean retention time for Bay K8644 was 3.030 minutes. Excellent linearity (r = 0.9998) was achieved in the range 0.10-1.40 µg/mL at 274 nm wavelength. Analytical limits were 16.56 ± 1.04 ng/mL for detection and 55.21 ± 3.48 ng/mL for quantitation respectively. Accuracy and precision studies showed good results (95-105%). Robustness was assessed by varying ±3%, both temperature and flow rate. Five different stress conditions were applied to assess Bay K8644's stability. Only basic and photolytic treatments yielded degradation products, both correctly resolved in a total runtime of 4 minutes. In conclusion, we developed a fast, simple, sensitive, accurate, precise, reliable and stability indicating method for detecting/quantifying Bay K8644, and tentatively characterized its main impurities/forced degradation products.

Effect of the incorporation of hydroxyapatite on the diametral tensile strength of conventional and hybrid glass ionomer cements.

The objective was to evaluate the effect of the incorporation of calcium hydroxyapatite particles (HAp) in the diametral tensile strength of a conventional type II glass ionomer (GC Gold Label 2) and a resin-modified glass ionomer cement (GC Gold Label 2 LC R). Two experimental HAp (E1HAp or E2HAp) were synthesized and characterized using X-ray diffraction and Confocal Raman spectroscopy. Both HAp were added into the powder of a conventional or resin-modified glass ionomer cement at 5 or 10 wt.%. A commercial HAp (CHAp) was used as reference material. For each glass ionomer cement, a group without the incorporation of HAp was used as a control. A universal testing machine was used for the mechanical test. The results were analyzed through a two-way ANOVA test followed by a complementary Tukey test. For all analyzes, the level of significance was set at α = 0.05. The average particle size for E1Hap was 15 µm, E2HAp was 35 µm and for CHAp was 1 µm. For conventional GIC, the addition of 10% E1HAp and 5% CHAp significantly increased the diametral tensile strength values (p ≤ 0.005). On the other hand, for the resin-modified GIC, except for the 5% E2HAp group, all experimental groups significantly reduced the values of diametral tensile strength (p ≤ 0.007). The addition of HAp improved the mechanical properties only for the conventional glass ionomer cement.

Docetaxel in chitosan-based nanocapsules conjugated with an anti-Tn antigen mouse/human chimeric antibody as a promising targeting strategy of lung tumors.

The aim of this work was to evaluate the physicochemical and biological properties of docetaxel (DCX) loaded chitosan nanocapsules (CS Nc) functionalized with the monoclonal antibody Chi-Tn (CS-PEG-ChiTn mAb Nc) as a potential improvement treatment for cancer therapy. The Tn antigen is highly specific for carcinomas, and this is the first time that such structure is targeted for drug delivery. The nanocapsules (Ncs), formed as a polymeric shell around an oily core, allowed a 99.9% encapsulation efficiency of DCX with a monodispersity particle size in the range of 200 nm and a high positive surface charge that provide substantial stability to the nanosystems. Release profile of DCX from Ncs showed a sustained and pH dependent behavior with a faster release at acidic pH, which could be favorable in the intracellular drug delivery. We have designed PEGylated CS Nc modified with a monoclonal antibody which recognize Tn antigen, one of the most specific tumor associated antigen. A biotin-avidin approach achieved the successful attachment of the antibody to the nanocapsules. Uptake studies and viability assay conducted in A549 human lung cancer cell line in vitro demonstrate that ChiTn mAb enhance nanoparticles internalization and cell viability reduction. Consequently, these ChiTn functionalized nanocapsules are promising carriers for the active targeting of DCX to Tn expressing carcinomas.

Physico-chemical and antilisterial properties of nisin-incorporated chitosan/carboxymethyl chitosan films.

The objective of this work was to investigate the effect of the addition of carboxymethyl chitosan on the structural properties and antilisterial activity of nisin-incorporated chitosan films. Chitosan and carboxymethyl chitosan solutions were prepared with different mass ratios and bacteriocin nisin was added (0, 1000 and 6000 IU/ml). Filmogenic solutions were cast, dried and their physico-chemical and antimicrobial properties were investigated. For the same chitosan/carboxymethyl chitosan mass ratio, the addition of NIS at 6000 IU/ml led to changes in the macro- and microstructure, as well as in physico-chemical properties of films. On the other hand, carboxymethyl chitosan had a plasticizing effect and enhanced the distribution of the bacteriocin within the biopolymer matrix. Moreover, nisin-incorporated blend films of chitosan and carboxymethyl chitosan were more effective against Listeria monocytogenes than their pure chitosan counterparts. This study showed that different formulations of nisin-incorporated composite films of chitosan and carboxymethyl chitosan may provide options for developing bioactive packaging to improve food safety.

Mechanical properties and electronic structure of edge-doped graphene nanoribbons with F, O, and Cl atoms.

In this study, we present the structural, electronic, and mechanical properties of edge-doped zigzag graphene nanoribbons (ZGNRs) doped with fluorine, oxygen, and chlorine atoms. To the best of our knowledge, to date, no experimental results concerning the mechanical properties of graphene-derived nanoribbons have been reported in the literature. Simulations indicate that Cl- and F-doped ZGNRs present an equivalent 2-dimensional Young's modulus E2D, which seems to be higher than those of graphene and H-doped ZGNRs. This is a consequence of the electronic structure of the system, particularly originating from strong interactions between the dopant atoms localized at the edges. The interaction between dopant atoms located at the edges is higher for Cl and lower for F and O atoms. This is the origin of the observed trend, in which E > E > E for all the analyzed ZGNRs.

Reduced Graphene Oxides: Influence of the Reduction Method on the Electrocatalytic Effect towards Nucleic Acid Oxidation.

For the first time a critical analysis of the influence that four different graphene oxide reduction methods have on the electrochemical properties of the resulting reduced graphene oxides (RGOs) is reported. Starting from the same graphene oxide, chemical (CRGO), hydrothermal (hTRGO), electrochemical (ERGO), and thermal (TRGO) reduced graphene oxide were produced. The materials were fully characterized and the topography and electroactivity of the resulting glassy carbon modified electrodes were also evaluated. An oligonucleotide molecule was used as a model of DNA electrochemical biosensing. The results allow for the conclusion that TRGO produced the RGOs with the best electrochemical performance for oligonucleotide electroanalysis. A clear shift in the guanine oxidation peak potential to lower values (~0.100 V) and an almost two-fold increase in the current intensity were observed compared with the other RGOs. The electrocatalytic effect has a multifactorial explanation because the TRGO was the material that presented a higher polydispersity and lower sheet size, thus exposing a larger quantity of defects to the electrode surface, which produces larger physical and electrochemical areas.

Toward the understanding of the molecular basis for the inhibition of COX-1 and COX-2 by phenolic compounds present in Uruguayan propolis and grape pomace.

Propolis and grape pomace have significant amounts of phenols which can take part in anti-inflammatory mechanisms. As the cyclooxygenases 1 and 2 (COX-1 and COX-2) are involved in said mechanisms, the possibility for a selective inhibition of COX-2 was analyzed in vitro and in silico. Propolis and grape pomace from Uruguayan species were collected, extracted in hydroalcoholic mixture and analyzed. Based on phenols previously identified, and taking as reference the crystallographic structures of COX-1 and COX-2 in complex with the commercial drug Celecoxib, a molecular docking procedure was devised to adjust 123 phenolic molecular models at the enzyme-binding sites. The most important results of this work are that the extracts have an overall inhibition activity very similar in COX-1 and COX-2, i.e. they do not possess selective inhibition activity for COX-2. Nevertheless, 10 compounds of the phenolic database turned out to be more selective and 94 phenols resulted with similar selectivity than Celecoxib, an outcome that accounts for the overall experimental inhibition measures. Binding site environment observations showed increased polarity in COX-2 as compared with COX-1, suggesting that polarity is the key for selectivity. Accordingly, the screening of molecular contacts pointed to the residues: Arg106, Gln178, Leu338, Ser339, Tyr341, Tyr371, Arg499, Ala502, Val509, and Ser516, which would explain, at the atomic level, the anti-inflammatory effect of the phenolic compounds. Among them, Gln178 and Arg499 appear to be essential for the selective inhibition of COX-2.

Tiroides ectópico parafaríngeo. A propósito de un caso / Parapharyngeal ectopic thyroid: A clinical case report

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Current trends in materials for dye sensitized solar cells.

Here, we intend to review those patents related with the technology of dye sensitized solar cells. In particular we discuss patents and papers that enable metal oxide layer to be more controllable and feasible for applications, and new and innovative dyes, sensitizers and electrolytes with promising features. Finally various methods were reviewed for fabricating semiconductor layers and complete DSSC devices focusing on the mass production of photovoltaic cells.

Mechanical properties of graphene nanoribbons.

Herein, we investigate the structural, electronic and mechanical properties of zigzag graphene nanoribbons in the presence of stress by applying density functional theory within the GGA-PBE (generalized gradient approximation-Perdew-Burke-Ernzerhof) approximation. The uniaxial stress is applied along the periodic direction, allowing a unitary deformation in the range of ± 0.02%. The mechanical properties show a linear response within that range while a nonlinear dependence is found for higher strain. The most relevant results indicate that Young's modulus is considerable higher than those determined for graphene and carbon nanotubes. The geometrical reconstruction of the C-C bonds at the edges hardens the nanostructure. The features of the electronic structure are not sensitive to strain in this linear elastic regime, suggesting the potential for using carbon nanostructures in nano-electronic devices in the near future.

A novel five-coordinate cadmium phenanthroline thiosulfate.

The structure of the novel cadmium phenanthroline thiosulfate poly[[(1,10-phenanthroline-kappa(2)N,N')cadmium(II)]-micro(3)-thiosulfato-kappa(3)S:S:O], [Cd(S(2)O(3))(C(12)H(8)N(2))](n), with a pentacoordinated Cd centre, is reported. It forms linear chains built up around a 2(1) axis and is isostructural with the known bipyridine homologue. The structure is also compared with a previously reported closely related monoaqua monohydrated phase, where the Cd(2+) cation is hexacoordinated. The incidence of weak C-H.O interactions in the determination of its general packing properties is discussed.