In general, inductively coupled plasma mass spectrometry (ICP-MS) food analysis requires numerous sample treatment steps that imply an increase of analysis time and the use of chemicals. In this study, the main objective was to evaluate the applicability of the direct analysis by ICP-MS to determine twelve elements (Al, As, Ba, Cd, Cr, Cu, Fe, Mn, Ni, Pb, Se and Zn) in tea and herbal beverages. Direct analysis method was compared with two other sample treatments: minimum treatment (acid dilution) and using a destructive method (microwave assisted digestion). Besides the lowest time of analysis, direct analysis provides a reliable response and agrees with the “green chemistry” principles. High sensitivity was also observed by low values of limits of detection and quantification, in general, below 2.5 µg L-1. The method accuracy was evaluated by spiked experiments and values ranged between 82 and 120%. Low values of coefficient of variation were also observed, 2 to 17%, for all analytes. The method exhibited applicability for commercial tea samples as well as for drinks made by herb infusion.

Introduction: The contribution of diet and treatment planning in the treatment of Chronic Kidney Disease (CKD) has been recognized as having a significant clinical impact if introduced early. Objective: determine the levels of carbohydrates, proteins, lipids, energy and energy density (ED) in an oral hospital diet prescribed to CKD patients, and to evaluate the adequacy of this diet with respect to dietary recommendations. Methods: Diets were collected in a Brazilian public hospital on two non-consecutive days of six different weeks. The carbohydrate, protein, and lipid (total, saturated, monounsaturated, polyunsaturated, linoleic, linolenic and trans fatty acids) contents were determined in a laboratory. The amount of energy and the ED of the diets were calculated using the correction factor Atware and by dividing the total energy of the diet by weight, respectively. Results and Discussion: About 14.3% of the diets produced for patients with CKD were analyzed. The average density of the diets was low (0.7 kcal/g). In terms of nutritional adequacy, the average lipid content (15%) and linolenic fatty acid content (0.4%) were below the recommendation, as was energy (23.4 kcal/kg/day). The average carbohydrate content (63.5%) and protein content (1.0 g/kg/day) exceeded the recommendations levels. Conclusion: The oral hospital diet prepared for patients with CKD were considered unbalanced, and an unfavorable clinical treatment for these patients.

Introducción: La contribución de la dieta y planificación del tratamiento en el tratamiento de la enfermedad renal crónica (ERC) ha sido reconocida por tener un impacto clínico significativo si introducida tempranamente. Objetivo: determinar los niveles de hidratos de carbono, proteínas, lípidos, energía y densidad de energía (DE) en una dieta hospitalaria oral recetada para los pacientes con ERC, y evaluar la adecuación de esta dieta con respecto a las recomendaciones dietéticas. Métodos: Las dietas fueron recogidas en un hospital público brasileño en dos días no consecutivos de seis semanas diferentes. Los contenidos de los hidratos de carbono, proteínas, y lípidos (totales, saturadas, monoinsaturadas, poliinsaturadas, ácidos grasos linoleico, linolénico y trans) fueran determinados en un laboratorio. La cantidad de energía y la DE de las dietas se calcularon utilizando el factor de corrección de Atware, dividiendo la energía total de la dieta en peso, respectivamente. Resultados y Discusión: Fueran analizadas cerca de 14.3% de las dietas producidas y servidas a los pacientes con ERC. La densidad media de las di etas fue baja (0,7 kcal/g). Fue encontrada inadecuación nutricional para el contenido medio en lípidos (15%) y contenido de ácido graso linolénico (0,4%) y de energía (23,4 kcal/kg/día). El contenido de carbohidratos (63,5%) y el contenido de proteínas (1,0 g/kg/día) superaron los niveles de recomendaciones. Conclusiones: La dieta hospitalaria oral preparada para los pacientes con enfermedad renal crónica se muestra desequilibrada y desfavorable para el tratamiento clínico de los pacientes.

Introduction: The levels of cadmium (Cd) and lead (Pb) in foods should be monitored as a function of health risks. Objective: To evaluate Cd and Pb levels in oral hospital diets and in an oral food complement (OFC) according to their respective consumption by patients, and to estimate the patient's exposition risk. Methods: The levels of Cd and Pb were determined by ICP-OES in samples of regular, blend, soft and renal diets and OFC, collected on 6 weekdays. About 14.3% of the diets and OFC served were analyzed. Results and discussion: 163 patients participated, with mean weights and ages of 62.7 kg and 56.5 years, respectively, the majority being men (59.5%). The mean Cd content consumed was greater for men fed the regular and blend diets and similar amongst the sexes for the soft diet. The consumption of Cd (max. 21.02 µg/day) was below the provisional tolerable monthly intake (PTMI). The mean Pb ingested (max. 199.49 µg/day) was similar amongst the sexes. The soft diet showed the highest Pb content in September/2010, whereas the other showed no variation according to season. In September/2010 and January/2011, the soft and regular diets associated with the OFC offered 207.50 and 210.50 µg/day of Pb, respectively. Conclusions: The combination of the diet with the OFC increased the risk of an excessive ingestion of Pb, and the vulnerability of the patients to an excessive exposition to Pb could be greater due to water and medications. It was concluded that whereas the calculated ingestion of Cd conformed to the PTMI, the Pb level and ingestion represented a risk to the health of the patients.

Introducción: Los niveles de cadmio (Cd) y plomo (Pb) en los alimentos deben ser controlados en función del riesgo para la salud. Objetivo: Evaluar los niveles de Cd y Pb en dietas hospitalarias orales y complemento alimentario oral (OFC) y sus ingestiones por pacientes, con estimativa del riesgo de exposición. Métodos: Los niveles de Cd y Pb se determinaron mediante ICP-OES en muestras de dietas regular, blanda, fluida, renal y OFC, recogidas 6 días non-consecutivos. Fueron analizados 14,3% de las dietas y OFC servidos. Resultados y discusión: 163 pacientes participaron, con pesos y edades medias de 62,7 kg y 56,5 años, respectivamente, en su mayoría varones (59,5%). La media de Cd consumida fue mayor entre hombres alimentados con dietas regular y fluida y similar entre los sexos para la blanda. El consumo de Cd (máx. 21,2 µg/día) estaba por debajo de la ingesta provisional mensual tolerable (IPMT). El contenido medio de Pb ingerido fue similar entre sexos (máx. 199,49 µg/día). La dieta blanda mostró mayor contenido de Pb en septiembre/2010, mientras que las otras no variaron según la temporada. En septiembre/2010 y enero/2011, las dietas regular y blanda asociadas al OFC aportaron 207,50 y 210,50 µg/día de Pb, respectivamente. Conclusiones: La combinación de la dieta con OFC aumentó el riesgo de ingestión excesiva de Pb. La vulnerabilidad de los pacientes a una exposición excesiva podría ser mayor en función del agua y medicamentos. La ingestión de Cd calculada cumple el IPMT, pero el nivel de Pb y su ingestión representan riesgo para los pacientes.

A composição de minerais foi investigada em 154 amostras de pólen apícola, provenientes de diferentes regiões do Brasil. A técnica de ICP OES foi utilizada para determinar Ca, Cu, Fe, K, Mg, Mn, Na, P, Se e Zn, após mineralização em sistema de microondas. Utilizando parâmetros instrumentais otimizados conseguiu-se boa exatidão e precisão na determinação simultânea dos minerais. Em geral, as amostras dos estados do Nordeste apresentaram teores de minerais mais elevados e produção constante durante o ano. Os minerais Mn, Se, Cu, Zn, Fe são os que poderiam ter maior contribuição na dieta, podendo atingir 70, 37, 27, 17 e 17%, respectivamente, da ingestão dietética diária recomendada no Brasil. A análise de componentes principais mostrou que Ca, Cu, Fe, K, Mg, Mn, Na, P e Zn podem ser usados na classificação do pólen nacional em função da origem geográfica. Os teores dos minerais variaram amplamente ao longo do ano.

The mineral composition of bee pollen was investigated in 154 samples from different Brazilian regions. Ca, Cu, Fe, K, Mg, Mn, Na, P, Se and Zn were determined by ICP OES after microwave mineralization. Employing optimized instrumental parameters, the method was shown to have a good precision and accuracy for the simultaneous determination of minerals. Overall, samples from the Northeastern states presented significantly higher amounts of minerals and showed constant production throughout the year. Manganese, Se, Cu, Zn and Fe were the elements that showed the greatest possible contributions to the diet, contributing with 70, 37, 27, 17 and 17%, respectively, of the Brazilian recommended daily intake. Principal component analysis (PCA) was applied to study geographic effects. The elements Ca, Cu, Fe, K, Mg, Mn, Na, P and Zn were important in explaining the classification of pollen according to their geographical origin. The mineral levels varied widely during the year.

In this work a fast method for the determination of the total sugar levels in samples of raw coffee was developed using the near infrared spectroscopy technique and multivariate regression. The sugar levels were initially obtained using gravimety as the reference method. Later on, the regression models were built from the near infrared spectra of the coffee samples. The original spectra were pre-treated according to the Kubelka-Munk transformation and multiplicative signal correction. The proposed analytical method made possible the direct determination of the total sugar levels in the samples with an error lower by 8% with respect to the conventional methodology.

O leite humano é a primeira fonte de nutrientes que uma criança necessita para seu crescimento nos primeiros meses de vida. Os teores de muitos elementos minerais podem variar devido a alguns fatores, como a genética, a nutrição materna, o período de lactação e também entre os grupos étnicos. O objetivo deste trabalho foi de validar o uso do método de digestão por via seca (cinzas) e a técnica de espectrometria de emissão (ICP OES) para a quantificação dos elementos minerais Ca, P, Na, k, Mg, Zn, Fe e Mn presentes em 151 amostras de leite materno procedentes de doadoras de bancos de leite humano de Marília, SP. Os valores obtidos para os elementos minerais (mg L-1) nas amostras de leite variaram entre: Ca=145 a 478; P=87 a 293; Fe=0,03 a 1,13; k=271 a 1159; Mg=14,8 a 60,0; Na=54 a 933 e Zn=0,38 a 5,82. Para o Mn, os resultados obtidos foram inferiores ao limite de quantificação do método (0,02 mg L-1). Os valores obtidos para precisão e exatidão do método (%) foram, respectivamente: Ca=1 e 96; P=1 e 98; Fe=4 e 83; k=1 e 99; Mg=1 e 97; Na=1 e 98; Zn=8 e 96; Mn=8 e 82. De acordo com os resultados obtidos, foi verificado que o método apresentou precisão e exatidão satisfatórias para todos os elementos estudados.

Human milk is the child's primary source of nutrients during its first months of life. Mineral element levels can vary according to several factors such as genetic, the mother nutritional status, lactation period and ethnicity. The objective of the present study was the validation of a dry-ashed digestion method and ICP OES technique which were used for quantification of mineral elements (Ca, P, Na, k, Mg, Zn, Fe and Mn) in 151 samples of human milk collected from mothers in the city of Marília, SP. Values (mg L-1) obtained ranged from Ca=145 to 478; P=87 to 293; Fe=0.03 to 1.13; k=271 to 1159; Mg=14.8 to 60.0; Na=54 to 933 e Zn=0.38 to 5.82. Mn was below the limit of quantification (0.02 mg L-1) for all analyzed samples. Method precision and accuracy (%) values were respectively: Ca=1 and 96; P=1 and 98; Fe=4 and 83; k=1 and 99; Mg=1 and 97; Na=1 and 98; Zn=8 and 96; Mn=8 and 82. Results indicate that precision and accuracy were satisfactory for all elements analyzed on the present study.

Avaliou-se os níveis de mercúrio total em amostras de peixes de água doce, procedentes de pesqueiros e pisciculturas de 39 regiões do estado de São Paulo. As espécies de peixes estudadas foram: pacu (Piaractus mesopotamicus), tilápia (Oreochromis niloticus), piauçu (Leoporinum sp), matrinxã (Brycon cephalus), tambaqui (Colossoma macropomum) e carpa (Cyprinus carpis). Foram avaliadas três metodologias de digestão de amostras para a determinação de mercúrio total, variando-se o volume de mistura sulfonítrica utilizada e a concentração do permanganato de potássio, sendo que o uso de 10mL de mistura sulfonítrica e solução de permanganato de potássio a 7% (m/v) na digestão da amostra foi a que forneceu as recuperações mais altas (96%), precisão de 1% e limite de quantificação de 0,3µg/kg. Após a validação do método, foram realizadas as determinações de teor de mercúrio total em 293 amostras de pescado, usando a técnica de espectrometria de emissão com fonte de plasma acoplado em gerador de hidretos. Os níveis médios de mercúrio encontrados variaram entre: tambaqui (0,0003-0,012mg/kg), carpa (0,063mg/kg), matrinxã (0,0003-0,074mg/kg), pacu (0,0003-0,078mg/kg), piauçu (0,0003-0,183mg/kg) e tilápia (0,0003-0,217mg/kg). Os resultados mostraram que nenhuma das amostras procedentes das diferentes regiões e diferentes pesque-pagues, apresentaram níveis de mercúrio total acima do permitido pela legislação brasileira, que é de 0,5mg/kg para pescado não-predador.

In this work, the levels of mercury were evaluated in samples of freshwater fish, coming from fishing-grounds and piscicultures of 39 regions of São Paulo State. The species of fish studied were: pacu (Piaractus mesopotamicus), tilápia (Oreochromis niloticus), piauçu (Leoporinum sp), matrinxã (Brycon cephalus), tambaqui (Colossoma macropomum) and carpa (Cyprinus carpis). Three digestion methodologies of sample were evaluated for the mercury determination, with variation of the volume of sulphonitric mixture utilized and the potassium permanganate concentration. After the validation method the determinations of mercury level were recorded in 293 samples of fish, using the technique of emission spectrometry with plasma coupled to an hydrides generator. The medium levels of mercury found were the following: tambaqui (0,0003-0,012mg/kg), carpa (0,063mg/kg), matrinxã (0,0003-0,074mg/kg), pacu (0,0003-0,078mg/kg), piauçu (0,0003-0,183mg/kg) and tilápia (0,0003-0,217mg/kg), and this last one presented the higher contamination rate. The results showed that none of the samples obtained from the different regions and fish-and-pay establishments presented mercury levels above the permitted limits of Brazilian legislation; 0,5mg/kg for non carnivorous fish.

A combinação da espectroscopia no infravermelho próximo (NIR) e calibração multivariada (método dos mínimos quadrados parciais - PLS) para a determinação do teor de proteína total em amostras de café cru, foi investigada. Os teores de proteína total foram inicialmente determinados usando-se como método de referência o de Kjeldhal, e, posteriormente foram construídos modelos de regressão a partir dos espectros na região do infravermelho próximo das amostras de café cru. Foram coletados 159 espectros das amostras de café cru utilizando um acessório de reflectância difusa, na faixa espectral de 4500 a 10000cm-1. Os espectros originais no NIR sofreram diferentes transformações e pré-tratamento matemático, como a transformação Kubelka-Munk; correção multiplicativa de sinal (MSC); alisamento (SPLINE); derivada primeira; média móvel e o pré-tratamento dos dados escalados pela variância. O método analítico proposto possibilitou a determinação direta, sem destruição da amostra, com obtenção de resultados rápidos e sem o consumo de reagentes químicos de forma a preservar o meio ambiente. O método proposto forneceu resultados com boa capacidade de previsão do teor de proteína total, sendo que os erros médios foram inferiores a 6,7%.

The combination of near infrared spectroscopy (NIR) and multivariate calibration using the partial least square - PLS method for the determination of the total protein level in raw coffee samples was investigated. The total protein levels were initially determined using the Kjeldhal method as the reference method. Regression models were built from the spectra in the NIR region of the raw coffee samples. Spectra of 159 samples were recorded, using an accessory of diffuse reflectance, in the range of 4500 and 10000cm-1 with 4cm-1 resolution. To the raw spectral data, different transformations and mathematical pretreatment such as Kubelka-Munk transformation; multiplicative sign correction (MSC); spline smoothing; first derivative and boxcar averaging were applied. The data was also preprocessed by scaling each column by its variance. The analytical method proposed is non invasive and the cost and time of analysis are very much reduced, making possible the fast and direct determination of the total protein content. The prediction error of protein levels given by the regression model were in average lower than 6.7%, indicating that this method is a good alternative for protein determination in raw coffee samples.

Com o objetivo de avaliar a qualidade de águas minerais, foram analisadas amostras, adquiridas em supermercados, de oito fontes localizadas no Estado de São Paulo entre agosto de 1999 e maio de 2000, com coletas trimestrais. Os resultados das análises físico-químicas mostraram que as amostras possuíam, em sua maioria, composição química dentro dos limites permitidos pela legislação brasileira, exceto quatro amostras, que apresentaram resultados na análise de cor acima de 5 unidades PtCo, uma amostra com pH fora da faixa recomendada de 4,0 a 9,0 e uma amostra com alcalinidade em hidróxidos em duas épocas de análise. Os resultados obtidos para as diferentes amostras variaram de acordo com as seguintes faixas: pH de 6,39 a 9,92, alcalinidade de 0,0 a 189,1mg L-1 de bicarbonato, dureza de 0,00 a 136,00mg L-1 de carbonato de cálcio, cor de 0,0 a 9,0 unidades de PtCo, turbidez de 0,00 a 2,00 FTU de turvação, sulfato de 0,00 a 55,67mg L-1, sulfeto de 0,00 a 0,002mg L-1, cloreto de 0,00 a 23,53mg L-1, fluoreto de 0,02 a 0,8mg L-1, alumínio de 0,01 a 0,09mg L-1, bário de 0,00 a 0,26mg L-1, cálcio de 0,53 a 28,35mg L-1, crômio de 0,00 a 0,01mg L-1, ferro de 0,00 a 0,03mg L-1, potássio de 0,39 a 3,27mg L-1, sódio de 0,53 a 97,29mg L-1, magnésio de 0,00 a 9,10mg L-1, manganês de 0,00 a 0,05mg L-1, zinco de 0,00 a 0,03mg L-1, chumbo de 0,00 a 0,01mg L-1 e lítio de 0,00 a 0,02mg L-1. Os elementos cádmio, cobre e cobalto apresentaram-se abaixo dos limites de detecção dos métodos.

Samples from eight different sources of mineral water from São Paulo State were purchased from August 1999 to May 2000 in order to evaluate the physical-chemical quality. In general, most samples were within the limits permited by the Brazilian legislation, except for four samples which showed color results above 5 PtCo units, one sample with pH outside the recommended range (pH 4 to 9) and one sample which presented hydroxide alkalinity in two different periods of sampling. The results varied according to the following ranges: pH from 6.39 to 9.92, alkalinity from 0.00 to 189.10mg L-1 de HCO3-1, hardness from 0.00 to 136.00mg L-1 carbonate of calcium, color from 0.0 to 9.0 units PtCo, turbidity from 0.00 to 2.00 FTU of turbidity, sulphate from 0.00 to 55.67mg L-1, sulfide from 0.00 to 0.002mg L-1, chloride from 0.00 to 23.53mg L-1, fluoride de 0.02 a 0.8mg L-1 aluminum from 0.01 to 0.09mg L-1, barium from 0.00 to 0.26mg L-1, calcium from 0.53 to 28.35mg L-1, chromium from 0.00 to 0.01mg L-1, iron from 0.00 to 0.03mg L-1, potassium from 0.39 to 3.27mg L-1, sodium from 0.53 to 97.29mg L-1, magnesium from 0.00 to 9.10mg L-1, manganese from 0.00 to 0.05mg L-1, zinc from 0.00 to 0.03mg L-1, lead from 0.00 to 0.01mg L-1 and lithium from 0.00 to 0.02mg L-1. The elements cadmium, copper and cobalt were below the limits of detection for the analytical methods.

Com este trabalho, objetivou-se avaliar a exposição do aplicador à calda de agrotóxico, durante pulverização na cultura da videira, com 4 diferentes pulverizadores. Os equipamentos avaliados foram um pulverizador semi-estacionário típico, um pulverizador de barras adaptado a uma barra semi-circular com os bicos voltados para cima, um turbopulverizador marca Hatsuta modelo café, com sistema de turbina adaptado para utilização na cultura da uva, e um turbo-pulverizador marca KO, modelo Jales, regulados pelos produtores. Para avaliação da exposição dérmica potencial (EDP) amostradores foram distribuídos sobre 22 partes do corpo do aplicador, que pulverizou uma calda contendo 3000 ppm do cátion Cu+2 durante 35 a 40 min. Em laboratório o Cu+2 foi recuperado e quantificado e a exposição calculada em função da concentração do cátion na calda. O pulverizador semi-estacionário proporcionou a maior EDP, seguido pela barra, turbo adaptado e pelo turbo original. A porcentagem do volume pulverizado que atinge o corpo do aplicador num mesmo período de tempo, foi mais que 89 vezes maior para o semi-estacionário, quando comparado ao turbo Jales e à barra adaptada, e 44 vezes maior quando comparado ao turbo adaptado. As áreas mais expostas do corpo foram mãos, cabeça e dorso para os tratorizados e a EDP foi alta em praticamente todas as regiões do corpo com o semi-estacionário. Aspectos da EDP em função do equipamento e da forma de utilização são discutidos.

The aim of present study was to evaluate the dermal exposure of pesticide applicator, during spraying in grapes crop, with 4 different sprayers. The equipments utilized were a typical semi-stationery sprayer, a boom sprayer adapted with a semi-circulate boom with the nozzle returned upward, an airblast sprayer utilized in coffee crop with turbine system adapted for grapes and a original airblast sprayer for grapes (KO, model Jales), regulated by the workers. For assessment of potential dermal exposure (PDE) of spray man, 22 sampling pads were attached to body parts of spray man applying a solution containing 3000 ppm of Cu+2 during 35 to 40 min. Copper was extracted and quantified in laboratory and the exposure was calculated considering the original concentration of the spray solution. The semi-stationery sprayer provided largest PDE, followed by the adapted boom sprayer, adapted airblast and original airblast sprayer. The carrier percentage reaching the spray man body in the same period of time was more than 89 times higher for semi-stationery when compared with the original airblast and the adapted boom and 44 times higher compared to the adapted airblast sprayer. The most exposed areas of the spray man body were the hands, head and back for sprayers adapted to tractor, and PDE was high in practically all the areas of the body with the semi-stationery equipment. Aspects of PDE related to equipment and the form of their use are discussed.