Resumo As plantas alimentícias não convencionais têm uma variedade de compostos bioativos com valor nutricional. O jaracatiá (Vasconcellea quercifolia) pertence à família Caricaceae e é uma alternativa dietética com uma excelente composição nutricional. Este estudo teve como objetivo caracterizar a composição nutricional da farinha de frutos verdes do jaracatiá (V. quercifolia), a fim de aplicá-la em um alimento funcional. Para isso, a farinha foi caracterizada em relação a macro e micronutrientes, fatores antinutricionais, pH, atividade da água e cor. Esta farinha apresentou teores de carboidratos de 22,31%; proteínas de 9,65%; fibra alimentar dietética de 32,80%; lipídios de 14,95%, dos quais 63,56% são ácidos graxos insaturados, especialmente ácido oleico; e cinzas de 9,10%, com maiores concentrações para potássio, cálcio e magnésio. Portanto, a farinha de V. quercifolia tem características nutritivas e pode ser utilizada como suplemento alimentar.

Abstract Non-conventional food plants have a variety of bioactive compounds with nutritional value. Vasconcellea quercifolia A. St.-Hil., belonging to the Caricaceae family, is a dietary alternative with excellent nutritional composition. This study aimed at characterizing the nutritional composition of mountain papaya (V. quercifolia) green fruit flour, in order to incorporate it in a functional food. For that purpose, the flour was characterized regarding its macro and micronutrients, anti-nutritional factors, pH, water activity, and color. This flour showed contents of carbohydrate of 22.31%; protein of 9.65%; dietary fiber of 32.80%; lipids of 14.95%, 63.56% of which are unsaturated fatty acids, especially oleic acid; and ash of 9.10%, with higher concentrations for potassium, calcium and magnesium. Therefore, V. quercifolia flour had good nutritional characteristics and might be used as supplementary food.

ABSTRACT Olive leaves are agro-industrial residues resulting from pruning and / or olive harvesting, and are used in animal feed, as an organic fertilizer and as a source of compound extraction for various applications. This study aimed to carry out the physicochemical characterization, main bioactive compounds and the fatty acid profile of olive leaves from the cultivars Frantoio, Koroneike, Manzanilha, Arbosana and Arbequina. Proximal composition, pH, titratable acidity, minerals by MIP OES, bioactive compounds were determined by spectrophotometry, oleuropein and tocopherols by high performance liquid chromatography and the fatty acid profile by gas chromatography. The olive leaves had a high content of fibers and proteins, the predominant minerals were potassium and calcium, in addition the olive leaves had a high content of bioactive compounds, mainly flavonoids and carotenoids and the cultivar Koroneike had a higher content of oleuropein compared to the others. In relation to tocopherols, α-tocopherol stood out from the other tocopherols with the maximum concentration (63436.79 mg.100g-1) measured in the cultivar Arbequina. In view of the results found, it is concluded that olive leaves are sources of macromolecules, bioactive compounds and fatty acids, which can be extracted and applied in the most diverse areas.

This paper describes the evaluation of the total concentration of Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, K, Mn, Pb e Zn and the bioaccessible fraction of Ba, Cu, Fe, Mn, Pb and Zn in samples of grape skins from different cultivars (Vitis Viníferas Tannat and Cabernet Sauvignon) by MIP OES. For the determination of total concentration, acid decomposition with a reflux system adapted to the digestion tubes in the oxidizing medium of HNO3 and H2O2 were used. The accuracy of the method was verified by recovery tests, whose values ranged from 80 to 120%, as well as through a comparative method in closed system. Bi, Cd and Cr showed values for total content below the LOD or below the values acceptable for health while Pb is higher than 0.2 mg kg-1, for both cultivars. To evaluate the bioacessible fraction, the gastrointestinal system was simulated using an in vitro procedure, and its performance was assessed considering the bioaccessible fraction (supernatant) and the non-bioaccessible fraction, whose sum should be closed to the total concentration, and the results obtained were between 81 and 120%. Both cultivars showed similar values for the bioaccessible fractions (~13.5 – 53% of the total content).

Resumo No presente trabalho, a técnica de espectrometria de emissão óptica com plasma induzido por micro-ondas foi empregada para determinar as concentrações de Al, Cd, Cu, Hg, Mg, Sb e Zn em amostras de peixes (bagre, tainha, traíra, pintado e corvina) e de Al, Ba, Ca, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sb, Ti e Zn em amostras de camarão-rosa (Farfantepenaeus paulensis). As amostras foram preparadas usando a decomposição ácida com o sistema de refluxo. Para as análises de peixes, fez-se a comparação de dois sistemas de introdução de amostras no plasma: a nebulização convencional e o sistema multimode . Para se obterem as melhores condições utilizando o sistema multimode, parâmetros, como a concentração de HCl e do agente redutor NaBH4, foram investigados. A exatidão do método foi avaliada através de análises de materiais de referência certificados e de testes de adição de analito. As recuperações obtidas foram satisfatórias para ambas as amostras. Para os peixes, os melhores resultados foram obtidos usando o sistema multimode e as concentrações encontradas (em mg kg-1) foram 6,43 a 24,7 para Al; 0,41 a 6,6 para Cu; 168,2 a 211,2 para Mg, e 23,1 para Zn. Para as amostras de camarão-rosa, as concentrações máximas (em mg kg-1) encontradas foram: 92,1 para Al; 1.070 para Ca; 4,57 para Cu; 87,9 para Fe; 451 para Mg; 8,9 para Mn, e 29,2 para Zn. Todas as concentrações de Cd, Cu, Pb e Zn encontradas estão dentro dos limites permitidos pela legislação vigente no Brasil, para pescados. Os resultados obtidos mostraram a adequabilidade do método utilizando a técnica de MIP OES para determinação multielementar em amostras de peixe e camarão-rosa.

Abstract In the present work, the microwave induced plasma optical emission spectrometry technique was employed to determine the concentrations of Al, Cd, Cu, Hg, Mg, Sb and Zn in fish samples (catfish, mullet, wolf fish, spotted sorubim and croaker) and Al, Ba, Ca, Cd, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sb, Ti and Zn in shrimp (Farfantepenaeus paulensis) samples. Samples were prepared by acid decomposition with reflux system. For fish analysis, two systems of sample introduction into plasma were compared: conventional nebulization and multimode system. In order to get the best conditions using the multimode system, parameters such as the concentrations of HCl and of reducing agent NaBH4 were investigated. The method accuracy was assessed through analysis of certified reference materials and analyte addition tests. The obtained recoveries were satisfactory for both samples. For fish, the best results were obtained using the multimode system and the maximum concentrations (in mg·kg-1) were: 6.43 to 24.7 for Al; 0.41 to 6.6 for Cu; 168.2 to 211.2 for Mg and 23.1 for Zn. For shrimp samples, the maximum concentrations (in mg·kg -1) were: 92.1 for Al; 1,070 for Ca; 4.57 for Cu; 87.9 for Fe; 451 for Mg; 8.9 for Mn and 29.2 for Zn. All concentrations found for Cd, Cu, Pb and Zn are within the limits permitted by the current legislation in Brazil for fish. The results showed the suitability of the present method using MIP OES technique for multielemental determination in fish and shrimp samples.

Resumo Neste trabalho, é descrito o desenvolvimento de um método analítico para análise de amostras de cervejas por técnicas de espectrometria. As amostras foram preparadas por decomposição em meio ácido, em um sistema de refluxo, e as determinações foram realizadas por F AAS (Fe, Mg e Zn), F AES (Na) e MIP OES (Ca, Fe, K, Mg, Mn, Na, Ni e Zn). As melhores condições para a decomposição da amostra foram obtidas através de estudo com delineamento composto central rotacional: volume de 10,0 mL de cerveja desgaseificada, adição de 5,0 mL de HNO3 e 2,0 mL H2O2, seguida por uma etapa de aquecimento em bloco digestor a 160 °C, por 93 min. Os limites de quantificação do método foram ≤ 0,100 mg L-1 para todos os elementos investigados, independentemente da técnica analítica utilizada, ficando abaixo, por exemplo, dos valores estipulados para Zn e Ni, pela Agência Nacional de Vigilância Sanitária do Brasil. Os estudos comparativos entre as diferentes técnicas avaliadas mostraram, pelo teste T com nível de 90% de confiança, que não há diferença significativa para as determinações de Fe, Mg, Na e Zn nas amostras de cerveja. O método de preparo da amostra proposto mostrou ser simples, rápido, de baixo custo e confiável, para análise de cervejas nas diferentes técnicas de espectrometria atômica.

Abstract This study describes the development of an analytical method for the analysis of beer samples by atomic spectrometric techniques. The samples were prepared by acid decomposition using a reflux system, and the determinations carried out by F AAS (Fe, Mg and Zn), F AES (Na) and MIP OES (Ca, Fe, K, Mg, Mn, Na, Ni and Zn). The best conditions for sample decomposition were obtained by way of studies using a central rotational compound design: 10.0 mL of degassed beer followed by the addition of 5.0 mL of HNO3 and 2.0 mL H2O2 and a heating step in the digester block at 160 °C for 93 min. The quantification limits of the method were ≤ 0.100 mg L-1 for all the analytes investigated, regardless of the analytical technique used, values below those established by the Brazilian Health Surveillance Agency for Zn and Ni, for example. The comparative study of the different techniques showed that, according to the t-test at a 90% level of confidence, there was no significant difference for the determinations of Fe, Mg, Na and Zn in the beer samples. The sample preparation method was shown to be simple, fast, low-cost and reliable for the analysis of beers by the different atomic spectrometry techniques.

This paper describes a sample preparation method for domestic ceramics, based on the acid decomposition assisted by ultrasound for further determination of Cu, Fe, Mg and Zn by Flame Atomic Absorption Spectrometry technique. The main optimized conditions were: particle size (25 µm); sample mass (25 mg) and the acid volume (0.5 mL of HNO3 and 0.5 mL of HF). The samples were placed in an ultrasonic bath for 2 hours at 40 ºC. The method was employed for eight commercial samples of domestic ceramic, which showed different concentrations for all analytes investigated, showing the existing variety of raw materials. The method showed good accuracy and precision, attested by the addition and recovery test, with values of 87 to 112% for all analytes and relative standard deviation lower than 3.0%.

This paper describes the evaluation of a new method of sample preparation using a cold finger system with continuous water flow for rice analysis by flame atomic absorption spectrometry. The limits of detection for Cu, Fe, Mn and Zn for the proposed method were 0.36, 1.84, 2.12 and 0.16 mg kg-1, respectively. The RSDs were lower than 6.0% for all elements and the CRM analyzed showed values with 95% agreement. The proposed method is simple and safe for the proposed objective and does not require the use of mixtures of acid or special equipment for sample preparation.

This paper describes the development of methods in micro-scale for the determination of K, Mg, Na and Zn in meat by atomic spectrometry techniques. The limits of detection (LOD) for K and Na by microdigestion were 0.18 and 0.20 mg g-1, respectively whereas LOD for Mg and Zn by microsolubilization with TMAH were 2.40 and 18.4 µg g-1, respectively. The RSD values were lower than 6.0% and the CRMs analyzed showed values with 95% agreement. The proposed methods are simple, fast and use small amounts of sample (around 10 mg) yet do not require special equipment for sample preparation.

In this review it is presented some aspects of electrothermal atomic absorption spectrometry with tungsten coil (ETAW-AAS) since its beginning until the present days as well as the perspectives for this technique. Some aspects concerning its development and theoretical concepts are discussed. The analytical figures of merit such as limit of detection (LD), characteristic mass (m0), relative standard deviation (RSD), accuracy and precision are evaluated, compared and discussed considering published works. It is also evaluated its advantages, applications, limitations and instrumental development. The use of diode laser as radiation source and its perspectives to ETAW are also discussed.