Alternativa analítica para especiação físico-química de mercúrio em águas costeiras tropicais

The determination of the physical-chemical mercury speciation in tropical coastal waters using the derivatization technique with CVAFS detection was optimized. This methodology is able to separate the elementary, reactive, organic and total mercury phases with low operational costs. The importance of bromide chloride solution, the diluted aqua regia, used as the oxidative solution, and different compositions of the reductive solution of stannous chloride were tested and the better results for coastal waters are presented. The recuperation of the sum of the different phases ranges from 80 to 94% of the total Hg content in duplicates of different marine samples. The optimized methodology permits important studies on the mercury cycle in the coastal environment.

Efeito do grau de moagem, do tipo de frasco e do volume vazio sobre a variabilidade analítica do fósforo extraído pelos métodos Mehlich-1 e Mehlich-3

Na execução de uma análise química de solo são empregados diversos procedimentos que, mesmo seguindo-se o protocolo preconizado pelo método de análise utilizado, estão sujeitos a variações nos resultados analíticos, causadas por manipulação das amostras ou dos materiais utilizados. Objetivou-se neste estudo avaliar a influência do grau de moagem da amostra, do tipo de frasco e do volume vazio no frasco na execução dos métodos Mehlich-1 e Mehlich-3 para determinar o P no solo. Para tanto, foram conduzidos três experimentos. No primeiro experimento, as amostras de solo foram moídas e tamisadas em peneiras com aberturas de 2,000; 1,700; 0,850; 0,600; e 0,300 mm. No segundo, foram utilizados dois modelos de frasco (erlenmeyer e snap-cap), ambos com volume de 50 mL. Já no terceiro, foi alterado o volume vazio no frasco, mantendo-se a relação solo:solução extratora utilizando-se as quantidades dentro do frasco de 1:10; 1,5:15; 2,5:25; 3:30; e 4:40 cm³ cm-3. O grau de moagem das amostras não influenciou a capacidade de extração do Mehlich-1; entretanto, a capacidade extrativa do Mehlich-3 foi influenciada, principalmente em solos argilosos. Tanto para o Mehlich-1 quanto para o Mehlich-3, os teores de P extraído foram significativamente mais elevados com o uso de frasco tipo snap-cap em relação ao erlenmeyer. O volume vazio no frasco alterou os teores de P extraído para o Mehlich-1 e Mehlich-3 em 100 e 64 % das amostras, respectivamente. Deve-se padronizar a intensidade da moagem das amostras de solo para extração do P pela solução de Mehlich-3. Um modelo único de frasco deve ser adotado pelos laboratórios de rotina para análise do P, independentemente do método de extração, mantendo-se sempre constante no frasco o volume da amostra (cm³) para o volume de solução extratora (cm³).

Determinação de Ácidos Carboxílicos na Atmosfera Urbana de São Paulo: uma abordagem analítica e ambiental

In this work, analytical strategies are evaluated in order to measure accurately the ambient levels of atmospheric organic acids. Environmental considerations about the determination of low molecular weight mono- and di-carboxylic acids from urban areas of São Paulo are described.

Metodologia analítica para a determinação de sulfato em vinhoto

In this way it is very important to know the sulfate concentration in vinasse samples before to make the biodigestor design. A previous developed and indirect method (Anal. Chim. Acta. 1996, 329, 197), was used to determine sulfate in samples of vinasse, after previous treatments, done in order to eliminate organic matter with hydrogen peroxide 30% and concentrated nitric acid mixture (3:1), under heating. Interferent cationic ions were isolated by using ion exchange columns. The results obtained for some samples from Araraquara and Penápolis are here presented. The phosphate concentration was also determined.

A quimiluminescência como ferramenta analítica: do mecanismo a aplicações da reação do luminol em métodos cinéticos de análise

Relevant aspects of proposed mechanisms of the chemiluminescent reaction of luminol are presented and commented to emphasize its perspectives for kinetic analysis. A careful search for analytical applications of this reaction is discussed in order to point out new trends of the studies. Kinetic analysis using the luminol reaction is proposed to be a very attractive due to the good performance of the reaction in analytical applications and the positive characteristics of kinetic analysis, such as low cost and sensibility. It is pointed out that kinetic analysis using the chemiluminescent reaction of luminol should be encouraged.

Avaliação da susceptibilidade magnética usando uma balança analítica

A simple system to measure the magnetic susceptibility of different materials is presented. The system uses an analytical scale with sensitivity on the order of micrograms and a permanent NdBFe magnet, based in the Rankine method. In this apparatus, the sample is placed near to the magnet that is fixed on the scale. Depending on the magnetic properties of the sample, an attractive or repulsive force will appear between the magnet and the magnetizing sample. Measuring this force, registered by the scale as a mass, the magnetic parameters such as: permeability and susceptibility of the sample can be determined. Despite it is simplicity the method is quantitative, precise and easily reproducible in many laboratories, what makes it attractive for teaching experiments.

Vitaminas lipossolúveis em alimentos: uma abordagem analítica

This study concerns certain problems inherent to the determination of fat-soluble vitamins in food, from extraction methods to identification and quantification. The discussion involves the main official and unofficial extraction methods coupled with spectrophotometric and HPLC techniques in which vitamins samples are obtained through liquid-liquid-solid and liquid-liquid-solid-solid extraction, indispensable to the analytical separation of different chemical compounds with vitamin functions. A saponification stage, possibly coupled with supercritical fluid extraction appears to be mandatory in the determination of vitamins A and E in their alcoholic forms. Alternative identification and quantification procedures are outlined: biological and chemical assays, analytical separations by HPLC (normal and reversed-phase), UV detection (all fat-soluble vitamins) and fluorescence detection (retinoids and tocopherols). Automation from sample preparation to quantification stages increases the data acquisition rate.

Validação de metodologia analítica para doseamento de soluções de lapachol por CLAE

Lapachol is a naphthoquinone found in several species of the Bignoniaceae family possessing mainly anticancer activity. The present work consists of the development and validation of analytical methodology for lapachol and its preparations. The results here obtained show that lapachol has a low quantification limit, that the analytical methodology is accurate, reproducible, robust and linear over the concentration range 0.5-100 µg/mL of lapachol.

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.

A evolução da balança analítica

This work intends to describe the historical evolution of the balance based on its technical improvement. This instrument has always been used for commercial and industrial purposes, but its value in research and chemistry was only recognized much later. The classical balance was the two-pan model for about 40 centuries, but when its importance in chemistry was established, particularly beginning at the end of the XVIIIth century, many improvements were made in order to increase sensitivity and shorten the weighing procedure. The balance design greatly changed along the XXth century: the classical two-pan models were replaced by one-pan balances that were replaced by electronic instruments.

Metodologia analítica para determinação de folatos e ácido fólico em alimentos

The aim of this work was to develop and to validate a methodology using HPLC for the simultaneous determination of folates and folic acid in foods. The limits of detection and the recovery rates for the vitamins in the certified reference materials were respectively 5 pg/mL and 94-108% for 5-MTHF, 7 pg/mL and 97-102% for THF, 30 pg/mL and 97.9-104% for 5-FTHF, 30 pg/mL and 95-107 for 10-FFA, 5 ng/mL and 97-102% for FA and 5 ng/mL and 98-103% for 10-MFA. Repeatability showed a coefficient of variation below 3.9% for all the vitamins. The proposed methodology was shown to be efficient when applied to different certified reference materials, namely pig's liver (BCR487), powdered milk (BCR421) and a vegetable mixture (BCR485).

Alquilbenzeno sulfonato linear: uma abordagem ambiental e analítica

The environmental impact of detergents and other consumer products is behind the continued interest in the chemistry of the surfactants used. Of these, linear alkylbenzene sulfonates (LASs) are most widely employed in detergent formulations. The precursors to LASs are linear alkylbenzenes (LABs). There is also interest in the chemistry of these hydrocarbons, because they are usually present in commercial LASs (due to incomplete sulfonation), or form as one of their degradation products. Additionally, they may be employed as molecular tracers of domestic waste in the aquatic environment. The following aspects are covered in the present review: The chemistry of surfactants, in particular LAS; environmental impact of the production of LAS; environmental and toxicological effects of LAS; mechanisms of removal of LAS in the environment, and methods for monitoring LAS and LAB, the latter in domestic wastes. Classical and novel analytical methods employed for the determination of LAS and LAB are discussed in detail, and a brief comment on detergents in Brazil is given.

Desenvolvimento e validação de metodologia analítica para determinação de itraconazol em produtos farmacêuticos por CLAE

Itraconazole is a synthetic antifungal drug administered orally with a broad spectrum of activity against mycotic infections. The present work consists of the development and validation of analytical methodology for evaluation of itraconazole in pharmaceutical products by high performance liquid chromatography. The separation was made using the reversed-phase column LC-18, acetonitrile/diethylamine 0.05% v/v, 60:40 v/v, pH 8.0 as mobile phase, methanol as solvent and detection and quantification at 254 nm. The results here obtained show that the analytical methodology is accurate, reproducible, robust and linear over the concentration range 8.0-12.0 µg/mL of itraconazole. The method was applied to pharmaceutical capsules containg itraconazole pellets and showed to be efficient, yielding good results.

Validação de metodologia analítica por cromatografia líquida para doseamento e estudo da estabilidade de pantoprazol sódico

Pantoprazole is a proton pump inhibitor used in the treatment of digestive ulcers, gastro-esophageal reflux disease and in the eradication of Helicobacter pylori. In this work, an analytical method was developed and validated for the quantification of sodium pantoprazole by HPLC. The method was specific, linear, precise and exact. In order to verify the stability of pantoprazole during dissolution assays, pantoprazole solution in phosphate buffer pH 7.4 was kept at room temperature and protected from light for 22 days. Pantoprazole presented less than 5% of degradation in 6 hours and the half live of the degradation was 124 h.

Validação de metodologia analítica para o doseamento simultâneo de mebendazol e tiabendazol por cromatografia líquida de alta eficiência

The aim of this work was to develop and validate an analytical methodology for simultaneous determination of mebendazole and thiabendazole, two benzimidazoles used as anthelmintics. The method was based on high performance liquid chromatography, using a C18 column, a mobile phase composed of KH2PO4 0.05 mol L-1 and methanol 40:60 (v/v) and UV detection at 312 nm. The results showed that the method presented linearity from 60.0 to 140.0 µg mL-1 for mebendazole and from 99.6 to 232.4 g µL-1 for thiabendazole and it was considered selective, accurate, precise and robust according to the specific resolution from ANVISA, the Brazilian regulatory agency.