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This paper proposes a closed inline system for decomposition of wine, aiming at the determination of lead using electrothermal atomization atomic absorption spectrometry (ETAAS). The system is built using a 0.8 mm diameter PTFE tube, which is wrapped around an 8 W UV lamp. The sample in the presence of 70% hydrogen peroxide is circulated on an 8 W UV lamp at the flow rate of 1 mL min-1 for 45 min. Under these conditions, the carbon content varied from 10% to 2% for a red wine sample before and after digestion, respectively. The system has allowed the determination of lead in wine samples using the analytical line 283.306 nm in the presence of aluminum as the chemical modifier and pyrolysis and atomization temperatures of 800 and 1800 °C, respectively. Then, lead can be quantified employing the external calibration technique with limits of detection 0.27 and quantification 0.89 µg L-1, and characteristics mass of 18 pg. The precision expressed by relative standard deviation (RSD%) was 2.13%, calculated using six replicates of a digested solution of a wine sample with the lead content of 16.35 µg L-1. For evaluation of the accuracy method, two wine samples were analyzed simultaneously by the method proposed and also by inductively coupled plasma mass spectrometry (ICP-MS). A statistical test demonstrated no significant difference between the means obtained by these two techniques. Also, experiments involving addition/recovery tests confirmed the method's accuracy. The system was employed for digestion and determination of lead in four Brazilian wine samples. The lead content varied from 2.19 to 43.48 µg L-1.

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The present work proposes a method for the direct determination of Al, Cu, Cr, Fe and Ni in Brazilian carbonated soft drinks by electrothermal atomic absorption spectrometry (ETAAS). Samples of different flavors packed in containers made of different materials (polyterephthalate ethylene and glass bottles, and aluminum and steel cans) were analyzed. The method was optimized by building up pyrolysis and atomization curves in sample medium and by evaluating the calibration approach. Under optimized conditions, recoveries in the range of 92-104% were obtained in the evaluation of method accuracy. The limits of quantification for Al, Cu, Cr, Fe and Ni were 2.3, 0.93, 0.17, 0.90 and 1.2 µg L(-1), respectively. Also, the impact of the material used in the packaging and flavor on the concentrations of each metal in the samples was evaluated. It was proved that neither flavor nor packaging material affected the concentrations of Al and Fe in the samples. On the other hand, the packaging material influenced the concentration of Cu, Cr and Ni, and only the flavor affected the concentration of Cu in the samples. These conclusions were based on the data obtained from the application of a two-way ANOVA evaluation at 95% confidence level.

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A highly sensitive and selective procedure for the determination of arsenate and total arsenic in food by electrothermal atomic absorption spectrometry after cloud point extraction (ETAAS/CPE) was developed. The procedure is based on the formation of a complex of As(V) ions with molybdate in the presence of 50.0 mmol L(-1) sulfuric acid. The complex was extracted into the surfactant-rich phase of 0.06% (w/v) Triton X-114. The variables affecting the complex formation, extraction and phase separation were optimized using factorial designs. Under the optimal conditions, the calibration graph was linear in the range of 0.05-10.0 µg L(-1). The detection and quantification limits were 10 and 33 ng L(-1), respectively and the corresponding value for the relative standard deviation for 10 replicates was below 5%. Recovery values of between 90.8% and 113.1% were obtained for spiked samples. The accuracy of the method was evaluated by comparison with the results obtained for the analysis of a rice flour sample (certified material IRMM-804) and no significant difference at the 95% confidence level was observed. The method was successfully applied to the determination of As(V) and total arsenic in rice samples.

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Arsenic is an element widely present in nature. Additionally, it may be found as different species in several matrices and therefore it is one of the target elements in chemical speciation. Although the number of studies in terrestrial plants is low, compared to matrices such as fish or urine, this number is raising due to the fact that this type of matrix are closely related to the human food chain. In speciation analysis, sample preparation is a critical step and several extraction procedures present drawbacks. In this review, papers dealing with extraction procedures, analytical methods, and studies of species conservation in plants cultivated in terrestrial environment are critically discussed. Analytical procedures based on extractions using water or diluted acid solutions associated with HPLC-ICP-MS are good alternatives, owing to their versatility and sensitivity, even though less expensive strategies are shown as feasible choices.

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Esta investigación trata sobre la determinación de germanio en exudado de hojas de zábila, mediante la técnica ana lítica espectrometría de absorción atómica con atomización electrotérmica (ETAAS). El exudado de las hojas de zábila es el líquido amarillo y de sabor amargo que emana de las hojas de la planta cortadas en la base. Es también conocido como zumo o látex. Ha sido utilizado en el tratamiento de diversas afecciones tales como: tratamiento de heridas, infecciones bucales, irritaciones de la piel, otras. El germanio es un oligoelemento que ha sido utilizado como inmunoestimulante y en pacientes con neoplasia. La concentración del germanio presente en el exudado de Aloe vera (L.) Burm.f. fue de 7.42 ± 2.33 μg/g. La metodología empleada fue validada por estudio de recuperación, ubicándose en un valor promedio de 97.43 ± 2.22%. La desviación estándar relativa fue de 2.88%, lo que es un indicativo de la precisión. El método utilizado para la determinación del elemento en cuestión es exacto, preciso y libre de interferencias.

The objective of this work was to determine the concentration of germanium in Aloe vera (zábila) from leaves exudated, using the electrothermal atomic absorption spectrometry analytical technic (ETAAS). The exudated is a yellow and bitter liquid, used in wounds healing, skin irritations, mouth infections, etc. The germanium is a trace element used as immunestimulant in patients with tumour. A concentration of 7.42 ± 2.33 μg/g was found. The method for the determination of germanium was validated by recovery studies, a value of 97.43 ± 2.22% was obtained for germanium, and the relative standar deviation (RSD%) was 2.88%. The method was exact, precise and free from interferences.

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En esta investigacion se estudio la concentracion de microelementos tales como cobre, zinc, manganeso y hierro en el acibar de hojas de zabila, por espectrometria de absorcion atomica en llama (FAAS); asimismo, la concentracion de cromo por espectrometria de absorcion atomica electrotermica (ETAAS). Las plantas fueron cultivadas en la ciudad de Coro, estado Falcon, Venezuela. Las muestras de aci bar se recolectaron en hojas internas, medias y externas de la planta. Luego, se secaron por liofilizacion y se mineralizaron: 0,25 g de muestra de acibar se sometio a digestion humeda por 1 hora a 70 oC en una plancha de calentamiento, con 1:2 HNO3 y H2O2. No se encontro efecto de matriz, ya que no hubo diferencia estadisticamente significativa entre la pendiente de la curva de calibracion acuosa y la obtenida por adicion de estandar. El estudio de recuperacion fue satisfactorio, siendo el valor promedio 97,02 ± 4,65%. La exactitud del metodo se evaluo utilizando material certificado de la National Bureau of Standards (NBS) 1572, no encontrandose diferencias estadisticamente significativas entre los valores de los metales contenidos en el material de referencia con los valores obtenidos con el metodo aplicado en esta investigacion. Con relacion a la precision, el promedio de la desviacion estandar relativa fue de 1,26%, lo que certifica la precision del metodo empleado. Las concentraciones de metales (media poblacional ± intervalos de confianza) encontradas fueron las siguientes: Cu: 1.604 ± 0.296 mg/g, zn: 6.381 ± 0.974 mg/g, Fe: 14.609 ±3.161 mg/g, Mn: 5.058 ± 0.307 mg/g y Cr: 13.174 ± 3.046 mg/g. El metodo empleado fue exacto, preciso y libre de interferencias.

In this investigation was studied the concentration of microelements such as: Cu, zn, Fe and Mn in Aloe vera (L.) Burm. f. leaves exudates by atomic absorption spectrometry (FAAS), also the Cr concentration was determined by electrothermal atomic absorption spectrometry (ETAAS). The plants were cultivated in Coro city, Falcon state, Venezuela. The exudates samples were recollected from internal external and intermediate leaves of the plant. It was digested for 1 hour in a hot plate at 70 oC 0.25g of lyophilized exudates with 1:2 nitric acidic and hydrogen peroxide. It was no found significatives statistics difference at 95% of confidence between the standard calibration curve and the aqueous calibration curve, so no matrix effect was observed. The recovery studies was satisfactory, the mean value was 97.02 ± 4.65%. It was no found significatives statistics differences at 95% of confidence between the certificated values from The National Bureau of Standards (NBS) 1572 of studied metals and the values found with the applied methodology, so the method applied was accurate. The precision of the method was 1.26%. The concentrations of these elements in the real samples were: Cu: 1,604 ± 0,296 mg/g; zn: 6,381 ± 0,974 mg/g; Fe: 14,609 ± 3,161 mg/g; Mn: 5,058 ± 0,307 mg/g and Cr: 13,174 ± 3,046 mg/g. The method used to determine these elements was exact, precise and free from interferences.

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El polen apícola es el segundo producto de la colmena más consumido, después de la miel de abejas; sin embargo, no tiene normas para su control de calidad en Venezuela. Los oligoelementos del polen han sido estudiados en sus funciones nutricionales, medicinales o tóxicas, y también como indicadores de contaminación ambiental mediante el análisis de metales pesados. En el presente trabajo se evaluó la concentración de Pb en polen apícola de Brassica napus L. producido en el estado Mérida. El análisis de Pb se realizó por espectroscopia de absorción atómica, con atomización electrotérmica (ETAAS). Se encontró una concentración de 268.31 ± 0.0008 µg Pb/kg de polen apícola fresco de Brassica napus L. El método para el análisis de plomo fue validado mediante estudios de recuperación, obteniéndose un valor de 101.0 ± 4,8%, con una desviación estándar relativa (RSD%) menor a un 5%, lo cual indica que el método empleado fue exacto, preciso y libre de interferencias.

Bee pollen is the second product of the comb most consumed, after honey; however, there are no regulations for its quality control in Venezuela. The oligoelements of pollen have been studied for their nutritional, medicinal or toxic functions, and also, as indicators of environmental pollution by the analysis of heavy metals. In this work, the concentration of Pb was evaluated in bee pollen of Brassica napus L. in the state of Mérida. The Pb analysis was done by electrothermal atomic absorption spectroscopy (ETAAS). A concentration of 268.31 ± 0.0008 µg Pb/kg fresh bee pollen of Brassica napus L. was found. The method for the analysis of lead was validated by recovery studies, a value of 101.0 ± 4,8% was obtained for lead, and the relative standard deviation (RSD%) was lower than 5%, indicating that the method was exact, precise and free of interference.