Especiação analítica de compostos de arsênio empregando métodos voltamétricos e polarográficos: uma revisão comparativa de suas principais vantagens e aplicações

This paper provides a review on voltammetric and polarographic methods for the speciation analysis of inorganic and organic arsenic compounds in different matrices. A discussion on the main advantages of electroanalytical methods in comparison with other analytical methods employed for arsenic speciation is presented. The mechanistic aspects of the most relevant techniques employing cathodic and anodic stripping voltammetry as well as polarographic methods published in the last twenty five years are summarized and discussed. The bibliographic references cited in this work were selected from the Web of Science (published by the ISI) and the main journals of analytical chemistry.

Métodos para análise de ácido clorogênico

This paper describes the analytical methods for determination of total chlorogenic acid (CGA) and their individual isomers. Spectrofotometric methods are adequate for total CGA analysis in green coffee but they can provide inflated results for coffee products. High pressure liquid chromatography (HPLC) with gel permeation column and ultraviolet (UV) monitoring is adequate for the simultaneous analysis of total CGA, alkaloids and sugars in coffee products. HPLC-UV-reversed phase is a simple, rapid and precise method for the determination of the individual isomers of CGA. Gas chromatography (GC) also is applied to the analysis of the individual isomers but phenolic acids need to be derivatized before analysis. Both HPLC- and GC-mass spectrometry provide an unequivocal identification of the individual isomers. The capillary electrophoresis method is simple, rapid and adequate to the simultaneous analysis of polyphenols and xanthines. Advantages and limitations of each method are discussed throughout the text.

Métodos de preparação de nanopartículas metálicas suportadas em carbono de alta área superficial, como eletrocatalisadores em células a combustível com membrana trocadora de prótons

Fuel cells are attracting much interest as efficient and clean energy conversion devices. The main components of low temperature fuel cells are the electrocatalysts used to promote the anodic and cathodic reactions, which are based on platinum and platinum alloys. These electrocatalysts are normally prepared in the form of metal nanoparticles supported on a conductive material, usually high surface area carbon, to improve catalyst utilization and reduce cost. This work presents and comments some methods used presently to produce these electrocatalysts. The performances of the produced electrocatalysts are compared to that of state-of-the-art commercial E-TEK electrocatalysts.

Validação em métodos cromatográficos e eletroforéticos

The validation of an analytical method is fundamental to implementing a quality control system in any analytical laboratory. As the separation techniques, GC, HPLC and CE, are often the principal tools used in such determinations, procedure validation is a necessity. The objective of this review is to describe the main aspects of validation in chromatographic and electrophoretic analysis, showing, in a general way, the similarities and differences between the guidelines established by the different Brazilian and international regulatory agencies.

Análise estrutural de ciclodextrinas: um estudo comparativo entre métodos teóricos clássicos e quânticos

In the present work, we analyzed the accuracy of distinct theoretical methods to reproduce the solid state structures of cyclodextrins. The a, b and g-cyclodextrins (CD) were considered and also their hydrates with included water molecules: a-CD.2H2O, b-CD.10H2O and g-CD.12H2O. The geometries were fully optimized using Molecular Mechanics (MM2), semiempirical (AM1 and PM3) and ab initio (HF/3-21G) methods and quantitatively compared with experimental data from X ray diffraction. The results obtained from the classical MM2 method were in best agreement with the experiment. The semiempirical and ab initio structures were also in satisfactory accordance with the experimental data. In general, the PM3 method was found to be more suitable than the AM1 to describe the CD geometries, mainly when the intramolecular hydrogen bonds are considered.

Métodos de obtenção e aplicações sintéticas de tiazóis, uma importante classe de compostos heterocíclicos

Thiazoles comprise an important class of heterocyclic compounds present in many potent biologically active molecules. This heterocyclic ring also shows various applications in organic synthesis to obtain new compounds. This paper presents different methodologies for the preparation of thiazole ring systems, as well as their synthetic applications.

Métodos imunoquímicos para análise de contaminantes ambientais: conceitos, estado da arte e perspectivas

Immunoassay techniques provide simple, powerful and inexpensive methods for analysis of environmental contaminants. However, the acceptance of immunoassays is dependent on the clear demonstration of quality and validity compared to more traditional techniques. In this review, primarily, the understanding and the fundamentals of immunoassay methods are given in order to make good use of immunoassays, especially of EIA tests. Special attention is given to the concepts related to the enzyme-linked immunosorbent assay (ELISA) formats, such as inhibition concentration at 50% (IC50), detection limit (LOD), cross-reactivity (CR %). It is also explained why some immunoassays are quantitative methods whereas others can only be used as screening methods. A list of main commercial kits for detection of priority pollutants is given in order to help analysts. Others formats, such as flow-injection immunoassay analysis (FIIA), immunoassay chromatography and immunosensors are also cited.

Teste de TBA aplicado a carnes e derivados: métodos tradicionais, modificados e alternativos

The TBA test is essential to quality control of fat-containing food, being the test most applied to evaluate lipid peroxidation in fishery, meat and poultry products. It estimates malonaldehyde, a secondary oxidation product, by reacting with 2-thiobarbituric acid, forming a coloured complex, measured spectrophotometrically atlambda = 532 nm. Results are expressed as mg malonaldehyde per kg sample or frequently as "TBA value". There are four ways of quantifying it: by lipid extraction, direct heating, distillation or heat-acid extraction. This review intends to point out traditional, modified and alternative TBA test methods, besides enumerating advantages and drawbacks of each one.

Síntese de indanos: uma seleção de métodos gerais e eficientes

The indan ring system is present in several compounds with important pharmacological properties. In this account recent examples of selected methods (Friedel-Crafts acylation, cycloaddition reactions, ring contraction, cyclization and resolution) for the synthesis of indans are discussed.

Diazepam e nordiazepam em plasma: métodos de extração líquido-líquido e em fase sólida no pré-tratamento de amostras para análise cromatográfica em fase líquida

Analysis of diazepam (DZP) and its active metabolite nordiazepam (NDZP) in plasma is commonly performed in clinical medicine to ensure proper therapeutic effects while minimizing the incidence of toxicity. This study aimed to optimize analytical parameters and compare two pre-treatment techniques, liquid-liquid (LLE) and solid phase extraction (SPE), as well as liquid chromatographic conditions to analyze simultaneously DZP and NDZP in plasma from 20 patients treated with a daily dose of 10 mg. Both techniques showed to be well in line with the international criteria for analytical validation, which permitted to quantify DZP (66.2 - 1148.6 ng mL-1) and NDZP (138.5 - 808.6 ng mL -1) in all samples. The correlation coefficients between SPE and LLE were respectively 0.9729 for DZP and 0.9643 for NDZP.

Los métodos alternativos en el estudio de la seguridad de cosméticos

El Reglamento 1223/2009 establece las normas que deben cumplir todos los productos cosméticos comercializados en Europa, con objeto de velar por el funcionamiento del mercado interior y lograr un elevado nivel de protección de la salud humana garantizando el uso de métodos alternativos que no impliquen la utilización de animales. El Laboratorio Europeo de Referencia para las Alternativas a la Experimentación con Animales (EURL-EURL- ECVAM) es el laboratorio de referencia en Europa encargado de validar los métodos alternativos. Posteriormente pueden ser homologados por la Organización de Cooperación y Desarrollo Económico (OCDE). Por otro lado, el Comité Científico de Seguridad de los Consumidores (SCCS) asesora a la Comisión sobre todos los temas relacionados con la seguridad de los cosméticos. En esta revisión se detalla una relación de métodos alternativos necesarios para evaluar la seguridad de los ingredientes cosméticos así como los métodos usados y sus limitaciones.

Métodos de reconocimiento del subsuelo

The aim of this workshop is to present the main methods of subsoil studies (namely mechanical and geophysical methods) to the Earth Sciences professorate. These methods frequently involve the use of specific material. The different methods are usually taught in the classroom where there is no real contact between the students and the equipment. Several activities, all of them taking place in surrounding areas of the university campus of Girona, will provide the assistants to the workshop with the opportunity of making measurements with different equipment. These activities will be made in the field so as to contribute to the resolution of a problem which will have been previously proposed. The problems presented are situations, most of them real, when subsoil investigation techniques are usually used. These cases have been employed as teaching-learning strategies with university and second grade students in the area of Girona. Finally, some examples of exercises involving the treatment of data obtained through subsoil investigation techniques are also presented to complement the workshop

Tiossemicarbazonas: métodos de obtenção, aplicações sintéticas e importância biológica

Thiosemicarbazones are a class of compounds known by their chemical and biological properties, such as antitumor, antibacterial, antiviral and antiprotozoal activity. Their ability to form chelates with metals has great importance in their biological activities. Their synthesis is very simple, versatile and clean, usually giving high yields. They are largely employed as intermediates, in the synthesis of others compounds. This article is a survey of some of these characteristics showing their great importance to organic and medicinal chemistry.

Los métodos alternativos en el estudio de la seguridad de cosméticos

El Reglamento 1223/2009 establece las normas que deben cumplir todos los productos cosméticos comercializados en Europa, con objeto de velar por el funcionamiento del mercado interior y lograr un elevado nivel de protección de la salud humana garantizando el uso de métodos alternativos que no impliquen la utilización de animales. El Laboratorio Europeo de Referencia para las Alternativas a la Experimentación con Animales (EURL-EURL- ECVAM) es el laboratorio de referencia en Europa encargado de validar los métodos alternativos. Posteriormente pueden ser homologados por la Organización de Cooperación y Desarrollo Económico (OCDE). Por otro lado, el Comité Científico de Seguridad de los Consumidores (SCCS) asesora a la Comisión sobre todos los temas relacionados con la seguridad de los cosméticos. En esta revisión se detalla una relación de métodos alternativos necesarios para evaluar la seguridad de los ingredientes cosméticos así como los métodos usados y sus limitaciones.

Adsorção de íons dicromato nos compósitos celulose/ZrO2.nH2O preparados pelos métodos da precipitação convencional e em solução homogênea

This article describes the preparation and characterization of the cellulose/ hydrated zirconium oxide composites prepared by conventional precipitation (PC) and homogeneous solution precipitation (PSH) methods. The composite obtained by the PC method was prepared by using an ammonia solution as the precipitating agent, while the composite obtained by the PSH method was prepared by using urea as the precipitating agent. The adsorption of dichromate ions on the composites was studied using factorial design 2³. The variables were: initial concentration, agitation time and mass of the composite. The data obtained agree better for the composite obtained by the PC method.