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Determination of Toxic Elements in Nuts by Inductively Coupled Plasma Mass Spectrometry after Microwave-Induced Combustion

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Abstract

Microwave-induced combustion (MIC) of nuts in closed vessels was evaluated as a sample preparation method for further determination of As, Cd, and Pb by inductively coupled plasma mass spectrometry (ICP-MS) and Hg by flow injection cold vapor generation coupled to ICP-MS (FI-CVG–ICP-MS). Conventional microwave-assisted acid digestion (MW-AD) in pressurized vessels was also used for results comparison. Samples were wrapped in polyethylene films and combusted using 20 bar of oxygen and 50 μl of 6 mol l−1 ammonium nitrate as aid for ignition. Sample masses up to 500 mg of hazelnuts, almonds, cashew nuts, Brazil nuts, and walnuts were combusted using 7 mol l−1 HNO3 as absorbing solution. Accuracy was evaluated using certified reference materials and an agreement better than 96% was obtained for all analytes. Using MIC, it was possible to obtain lower limits of detection (LODs) in comparison with those obtained by MW-AD. The LOD obtained using MIC was 3, 2, and 6 ng g−1 for As, Cd, and Pb, respectively. The LOD for Hg by FI-CVG–ICP-MS was 7 ng g−1. Residual carbon content obtained after decomposition by MW-AD and MIC was 20% and lower than 1.5%, respectively, showing the high efficiency of MIC and allowing the determination of toxic elements in samples with high fat content. With the use of MIC up to eight samples could be processed simultaneously and only diluted nitric acid was required minimizing physical interferences, reagent consumption, and waste generation.

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Acknowledgments

The authors are grateful to Conselho Nacional de Desenvolvimento Científico e Tecnológico and Coordenação de Aperfeiçoamento de Pessoal de Nível Superior for financial support and Instituto Nacional de Ciência e Tecnologia de Bioanalítica, Campinas, SP, Brazil.

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Authors and Affiliations

  1. Departamento de Química, Universidade Federal de Santa Maria, 97105-900, Santa Maria, Rio Grande do Sul, Brazil

    Aline L. H. Muller, Cristiano C. Muller, Fernanda Lyra, Paola A. Mello, Edson I. Muller & Erico M. M. Flores

  2. Instituto de Química e Geociências, Universidade Federal de Pelotas, 96010-610, Pelotas, Rio Grande do Sul, Brazil

    Marcia F. Mesko

Authors
  1. Aline L. H. Muller
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  2. Cristiano C. Muller
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  3. Fernanda Lyra
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  4. Paola A. Mello
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  5. Marcia F. Mesko
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  6. Edson I. Muller
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  7. Erico M. M. Flores
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Correspondence to Erico M. M. Flores.

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Muller, A.L.H., Muller, C.C., Lyra, F. et al. Determination of Toxic Elements in Nuts by Inductively Coupled Plasma Mass Spectrometry after Microwave-Induced Combustion. Food Anal. Methods 6, 258–264 (2013). https://doi.org/10.1007/s12161-012-9381-y

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  • DOI: https://doi.org/10.1007/s12161-012-9381-y

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