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The microwave-assisted digestion of dietary supplements using diluted nitric acid under oxygen pressure for subsequent indirect determination of phosphorus and sulfur by ion chromatography (IC) was proposed. Different concentrations of nitric acid (from 1 to 14.4 mol L−1) and oxygen pressures (from 5 to 20 bar) were evaluated. Dissolved organic carbon and residual acidity were used to choose the most suitable digestion condition. Using the proposed method, it was possible to digest up to 1350 mg of dietary supplements using only 5 mol L−1 HNO3 under 5 bar of oxygen pressure. Comparing to conventional digestion procedure it was possible to digest up to 60% higher sample mass using HNO3 around 30% more diluted. Recoveries ranging from 96 to 102% were obtained when recovery tests using a standard solution or a mixture with certificate reference material were carried out. The concentration of P and S indirectly determined by IC agreed with the results obtained by conventional microwave-assisted digestion using concentrated HNO3 and subsequent determination by inductively coupled plasma optical emission spectrometry. Keywords: Sample preparation, Digestion under oxygen pressure, Diluted acid, Ion chromatography, Food safety, Routine analysis

In this study, the microwave-induced combustion (MIC) method was evaluated for the sample preparation of the most consumed mushroom species in Brazil (Champignon, Shiitake, and Shimeji) and further halogen determination by ion chromatography (IC). For this, sample mass, combustion aid mass, and absorbing solution (H2O and 50 mmol·L−1, 100 mmol·L−1, or 150 mmol·L−1 NH4OH) were evaluated. Bromine and iodine concentrations, determined by IC, were lower than the limits of detection (LODs, Br: 6 mg·kg−1 and I: 24 mg·kg−1). Inductively coupled plasma mass spectrometry (ICP-MS) was also used for Br and I determination, and the LODs were lower (Br: 0.066 mg·kg−1 and I: 0.014 mg·kg−1) than those obtained by IC. Concentrations of Cl, obtained by IC, ranged from 523 mg·kg−1 to 13053 mg·kg−1 with LOD of 40 mg·kg−1. In turn, Br and I concentrations, obtained by ICP-MS, ranged from 2.49 mg·kg−1 to 5.50 mg·kg−1 and from

(1) Background: Elevated atmospheric CO2 concentration affects the growth and development of the rice crop. In Southern Brazil, rice is traditionally produced with continuous irrigation, implying a significant amount of water used. Besides, continuous flooding favors the uptake of toxic elements such as arsenic (As) and cadmium (Cd). In this work, one Brazilian rice cultivar (IRGA 424) was tested for the effects of elevated CO2 concentration and different water regimes on rice yield, and As and Cd accumulation in grain. (2) Methods: Rice was grown in two CO2 concentrations (400 and 700 µmol mol−1) and two irrigation regimes (continuous and intermittent). It was evaluated the number of tillers, plant height, aboveground dry weight (ADW), water use efficiency (WUE), rice yield components, and As and Cd concentration in rice grain. (3) Results: Rice plants were taller and had a higher WUE when cultivated at e[CO2]. The ADW and the rice yield component were not affected by CO2 levels nor water regimes. Intermittent flood regimes had a lower average As concentration. The Cd concentration in the samples in both growing seasons and all treatments was below the limit of quantitation (8.76 μg kg−1). (4) Conclusions: Enhanced CO2 concentration did not affect rice yield, increased the WUE, and reduced As concentration in grains. Regarding water management, the intermittent regime enhanced WUE and promoted a reduction in As concentration in grains.

A method based on microwave-induced combustion (MIC) was applied for the decomposition of different types of edible seaweed (Nori, Hijiki and Wakame) for subsequent determination of bromine and iodine by inductively coupled plasma mass spectrometry (ICP-MS). Decomposition of 500 mg of each sample was achieved in less than 30 min. A single and diluted solution (150 mmol L-1 (NH4)2CO3) was used for the absorption of both analytes and a reflux step of 5 min was applied to improve analyte recoveries. Accuracy was evaluated using certified reference materials and agreement was between 103 and 108% for both elements.

A novel solution-based calibration method for quantitative spatial resolved distribution analysis (imaging) of elements in thin biological tissue sections by LA-ICP-MS (laser ablation inductively coupled plasma mass spectrometry) is described. A dual flow of the carrier and nebulizer gas is used to transport the aerosol of the laser ablated solid sample (brain tissue) and that of the nebulized aqueous standard into inductively coupled plasma (ICP) source, respectively. Both aerosols are introduced separately in the injector tube inside a special ICP torch and then mixed in the inductively coupled plasma. Calibration curves were obtained viatwo different calibration strategies: (i) solution based calibration and (ii) with a set of well characterized homogeneous brain laboratory standards. In the first approach matrix matching is performed by solution nebulization of a series of aqueous standards with defined analyte concentrations and simultaneous laser ablation of brain homogenate followed by nebulization of 2% (v/v) HNO3and laser ablation of a whole brain slice (line by line). In the second approach of calibration a set of brain homogenates with defined analyte concentrations is analyzed by LA-ICP-MS followed by the imaging of brain tissue under the same experimental conditions (dry plasma). Calibration curves of elements of interest (e.g., Li, Na, Al, K, Ca, Ti, V, Mn, Ni, Co, Cr, Cu, Zn, As, Se, Rb, Sr, Y, Cd, Ba, La, Ce, Nd, Gd, Hg, Pb, Bi and U) were obtained using (i) aqueous standards or (ii) the set of synthetic laboratory standards prepared from a mouse brain homogenate doped with elements at defined concentrations. The ratio of the slope of the calibration curves (obtained by using aqueous standards and solid standards) was applied to correct the differences of sensitivity among ICP-MS and LA-ICP-MS. Quantitative images of Li, Mn, Fe, Cu, Zn and Rb in mouse brain were obtained under wet plasma condition (nebulization of HNO3solution in parallel with ablation of solid brain sample). [ABSTRACT FROM AUTHOR]

This paper describes the studies performed with the candidate Certified Reference Material (CRM) of captopril, the first CRM of an active pharmaceutical ingredient (API) in Brazil, including determination of impurities (organic, inorganic and volatiles), homogeneity testing, short- and long-term stability studies, calculation of captopril content using the mass balance approach, and estimation of the associated measurement uncertainty.Este artigo descreve os estudos realizados com o candidato a Material de Referência Certificado (MRC) de captopril, primeiro MRC de fármacos no Brasil, incluindo a determinação de impurezas (orgânicas, inorgânicas e voláteis), testes de homogeneidade, testes de estabilidade de curta e longa duração, cálculo do teor de captopril por balanço de massa e estimativa da incerteza de medição associada ao valor certificado.

This paper describes the validation of a reversed-phase high performance liquid chromatography method (RP-HPLC) with diode array detection (DAD) for determination of related substances (impurities from organic synthesis and degradation products) of captopril according to the Brazilian Pharmacopeia IV. The aim of this study was to guarantee the method accuracy for quantification of related substances, an essential requisite to determine, using the mass balance approach, the captopril content in the first Brazilian certified reference material (CRM) of an active pharmaceutical ingredient (API), developed by Inmetro. The captopril instability in solution is discussed and the captopril content determined by mass balance is compared to the results from titration and differential scanning calorimetry (DSC).Este artigo descreve a validação de método de cromatografia líquida de alta eficiência em fase reversa (CLAE-RP) com detector de fotodiodos (DAD) para determinação de substâncias relacionadas (impurezas orgânicas de síntese e produtos de degradação) de captopril segundo Farmacopéia Brasileira IV ed. Este estudo teve como objetivo garantir que o método é capaz de quantificar com exatidão o teor de substâncias relacionadas, um requisito essencial para que o teor de captopril seja determinado por balanço de massa no primeiro material de referência certificado (MRC) de fármacos brasileiro, o qual foi desenvolvido pelo Inmetro. A instabilidade do captopril em solução é discutida em detalhes e o teor de captopril determinado por balanço de massa é comparado com aqueles obtidos por titulação e por calorimetria exploratória diferencial (DSC).