A espectrometria atômica e a determinação de elementos metálicos em material polimérico

Polymeric materials are widely used in the chemical industry and are part of our daily lives. Inorganic species may be added to them as additives, anti-oxidizing agents, stabilizers, plasticizers, colorants and catalysts and may be present in a wide range of concentrations. Their determination demands the development of analytical methods considering different kinds of polymeric materials, their composition and the final use of the material. Although many different analytical techniques may be used, this review emphasizes those based on atomic absorption and emission spectrometry. Solid sampling techniques and digestion methods are described and discussed and compared considering published results.

Avaliação do efeito da concentração de carbonato na eletrodeposição de cobre sobre discos de aço-carbono

Mild steel blankets were covered with electrolytic copper thin layer, from cyanide bath, being evaluated the influence of the carbonate concentration in the physiochemical properties of those deposits. The cell voltage decreased as the current intensity decreased, but the adherence of the deposit was not enhanced, showing that the increment of carbonate concentration causes substantial problems. Chemical solubilization reactions of air-bearing carbon dioxide and oxidation of free cyanide ions through dissolved oxygen evolved in the anodic processes contribute to the copper plating to occur in an inefficient way. The best optimal conditions require a carbonate concentration below 50 g L-1.

Desenvolvimento e validação de um método analítico rápido por cromatografia líquida de alta eficiência para determinação de nimesulida em estudos de liberação in vitro

A high performance liquid chromatography (HPLC) method has been developed for a rapid determination of nimesulide in dissolution studies. Nimesulide was analyzed using 5 µm Lichrospher® RP-18 column (125 x 4 mm i.d.) and mobile phase acetonitrile: phosphate buffer pH=6.0 (55:45) at a flow-rate of 1.0 mL min-1. Detection was carried out at 300 nm at 25 ºC. The method was applied to analysis of nimesulide in in vitro release studies and showed a rapid and efficient analytical alternative for evaluation of dissolution profile of nimesulide.

A formação em Química discutida com base nos modelos proposto por estudantes de pós-graduação para o fenômeno de dissolução

Mental models play an important role in the evolution of an individual's so-called knowledge. Using such representations, students can explain, foresee, and attribute causality to observed phenomena. In the case of Chemistry, the ability to work mentally with models assumes great importance, due to the microscopic component that is characteristic of this science. With the objective of exploring students' ability to work with models, 27 students of the Chemistry Institute of UNESP were asked to describe the mechanisms of dissolution, in water, of NaCl, HCl and HCN, as well as the partial dissolution of I2. Due to difficulties of access to complex descriptors of these processes, each student was asked to explain the phenomena using words and drawings. The results of these investigations were analyzed, and enabled construction of a framework representing the Chemistry students' theoretical training, especially with respect to their most important transferred skill: an ability to model the physical world.

Validation of a simple and rapid UV spectrophotometric method for dexamethasone assay in tablets

This work reports the validation of an analytical UV spectrophotometric method to assay dexamethasone in tablets (assay and dissolution studies). The method was linear in the range between 1 and 30 µg mL-1 presenting a good correlation coefficient (r = 0.9998, n = 7). Precision and accuracy analysis showed low relative standard deviation (< 2.00%) and good percentual recoveries (95-105%). The procedure was linear, accurate, precise, and robust. The method is simple, and it has low cost. It does not use polluting reagents and can be applied in dissolution studies, being an adequate alternative to assay dexamethasone in tablets.

High encapsulation efficiency of sodium alendronate in eudragit S100/HPMC blend microparticles

The hydrophilic drug sodium alendronate was encapsulated in blended microparticles of Eudragit® S100 and Methocel® F4M or Methocel® K100LV. Both formulations prepared by spray-drying showed spherical collapsed shape and smooth surface, encapsulation efficiencies of 85 and 82% and mean diameters of 11.7 and 8.4 µm, respectively. At pH 1.2, in vitro dissolution studies showed good gastro-resistance for both formulations. At pH 6.8, the sodium alendronate release from the microparticles was delayed and was controlled by Fickian diffusion. In conclusion, the prepared microparticles showed high encapsulation efficiency of sodium alendronate presenting gastro-resistance and sustained release suitable for its oral administration.

Formulações de atrazina em xerogéis: síntese e caracterização

In this study, controlled release formulations of Atrazine (ATZ) were synthesized by the sol-gel method and characterized by elemental, FTIR, SEM, BET and DSC analyses. The release kinetic of ATZ from the formulations in CaCl2 0.01 mol L-1 medium was monitored by UV/Vis spectroscopy. In all formulations, ATZ was physically dispersed on the Si-polymer, and the dispersion grade decreased with increasing amount of herbicide. The ATZ release kinetics was controlled mainly by dissolution, and the data could be fitted to the Korsmeyer - Pepper model. The ATZ as xerogel presents a lower affinity for soil than as granulated form.

Tribocorrosão da liga TI6AL4V em solução salina tamponada com fosfato

The tribocorrosion behavior of Ti6Al4V alloy was investigated in a Phosphate Buffered Saline (PBS) solution by a reciprocating wear, using alumina ball as the counterface material, at different normal forces and sliding velocities. Dry wear experiments were performed in order to compare with the tribocorrosion experiments at open circuit potential and under anodic polarization. Dry wear induced a superior damage on the counterface, forming larger and shallower wear tracks compared with those experiments performed in PBS solution. The anodic current was increased by wear; however the volume of oxidized metal in tribocorrosion experiments correspond to a relative low percentage of the wear track volume.

Determinação de citrato de sildenafila e de tadalafila por cromatografia líquida de ultraeficiência com detecção por arranjo de diodos (CLUE-DAD)

A simple ultra-performance liquid chromatographic method for the simultaneous determination of sildenafil citrate and tadalafil was developed and validated. Sample preparation was dissolution in methanol, followed by centrifugation and dilution (1:10) with methanol. Analysis was performed in an Acquity® UPLC system with Acquity® BEH C18 column (2.1 x 50 mm, with 1.7 μm particles). The elution was isocratic with phosphate buffer pH 2.3 and acetonitrile (65:35, v/v) at a flow rate of 0.7 mL/min. The method presented adequate specificity, linearity, precision and accuracy and allowed the determination of the drugs in seized forensic samples.

Desenvolvimento e validação de um método analítico simples e rápido por espectroscopia UV para quantificação de aciclovir em matrizes hidrofílicas de liberação prolongada

This work reports the validation of an analytical UV spectrophotometric method to assay acyclovir in hydrophilic matrices (assay and dissolution studies). The method was linear in the range between 2.5-20 µg mL-1, presenting a good correlation coefficient ( r = 0,9999). Precision and accuracy analysis showed low relative standart deviation (< 2.0 %) and a good recoveries percentual (98.9-100 %). The procedure was linear, accurate, and robust. The method is simple and cheap. It does not use polluting reagents and can be applied in dissolution studies, being an adequate alternative to assay acyclovir in hydrophilic matrices tablets.

Electrochemical and theoretical evaluation of the interaction between dna and amodiaquine: evidence of the guanine adduct formation

The electrochemical behavior of the interaction of amodiaquine with DNA on a carbon paste electrode was studied using voltametric techniques. In an acid medium, an electroactive adduct is formed when amodiaquine interacts with DNA. The anodic peak is dependent on pH, scan rate and the concentration of the pharmaceutical. Adduct formation is irreversible in nature, and preferentially occurs by interaction of the amodiaquine with the guanine group. Theoretical calculations for optimization of geometry, and DFT analyses and on the electrostatic potential map (EPM), were used in the investigation of adduct formation between amodiaquine and DNA.

Comparação da labilidade de metais empregando voltametria, difusão em filmes finos por gradiente de concentração (DGT) e modelo computacional

Speciation of metals in a synthetic freshwater was comparatively evaluated using Anodic Stripping Voltammetry, Diffusive Gradients in Thin Films and a Chemical Equilibrium Model. The labile fractions of Cu and Zn quantified by DGT were similar to the ones measured by ASV. The labile species of Cd and Pb could not be determined by both experimental methods due to the formation of inert complexes with organic ligands in the sample. Despite the differences among the methods, the speciation results obtained by the use of DGT and ASV agreed well with predictions made by the chemical equilibrium model.

Development and validation of an UV spectrophotometric method for the determination of aliskiren in tablets

For determination of aliskiren in commercial samples, an analytical UV spectrophotometric method was developed and validate according to ICH guideline. The method was linear in the range between 40 and 100 μg mL-1 (r² = 0.9997, n = 7) and exhibited suitable specificity, accuracy, precision, and robustness. It is simple, it has low cost, and it has low use polluting reagents. Therefore, the proposed method was successfully applied for the assay and dissolution studies of aliskiren in tablet dosage forms, and the results were compared to a validated RP-LC method, showing non-significant difference (P > 0.05).

Encapsulation and release characteristics of glibenclamide loaded calcium-alginate beads

The aims of this study were to formulate calcium-alginate beads containing glibenclamide, characterize the resulting microparticles, evaluate the release characteristics of this type of delivery system in an in vitro dissolution test, and compare it with two commercially available trademarks (Daonil® and Glibetab®). We obtained glibenclamide loaded calcium-alginate beads with a rough surface and a particle size between 150-200 µm. For the in vitro dissolution test Daonil® at 45 min showed a Q > 70%, whereas Glibetab® and glibenclamide calcium-alginate beads a Q < 70%; in spite of that glibenclamide calcium-alginate beads showed significant release properties.

Validación de un método analítico empleando cromatografía líquida de alta eficiencia para la determinación de ibuprofeno en medios biorrelevantes

An analytical method by liquid chromatography has been proposed and validated to study the apparent solubility of ibuprofen in biorelevant dissolution media. The main properties of the studied media were pH values of 5.0 and 6.5 and the presence or absence of some natural surfactant agents. The parameters evaluated were specificity, linearity, precision, accuracy, and detection and quantification limits, as well as the drug stability under the analysis conditions. The developed method was useful to determine the apparent solubility of this drug as a function of temperature and surfactants concentration to demonstrate the validity of the Biopharmaceutics Classification System.