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Evaluation of Sample Preparation Methods for the Determination of Ca, Cu, Fe, K, and Na in Milk Powder Samples by ICP-OES

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Abstract

In this paper, a comparative study between three acid decomposition procedures of milk powder samples for the determination of Ca, Cu, Fe, K, and Na by optical emission spectrometry with inductively coupled plasma is presented. Utilizing a reflux system, it was possible to increase the temperature of the digester block above the boiling point of the reaction medium, avoiding the loss of analyte and the excessive evaporation of the acids during the heating. Conditions of acidity (10 mL HNO3/H2SO4), temperature (350 °C), and decomposition time (4 h) were defined by evaluation of residual carbon content. Acid digestion in an open system with a cold finger was compared with a conventional open system (4 h ate 120 °C), as well as with microwave digestion (heating ramp to 180 °C by the time 45 min), for four commercial samples of milk powder. For the three sample preparation procedures, the values of the analyte concentrations in all analyzed samples were similar. The accuracy of the acid digestion procedures for Ca, Cu, Fe, K, and Na was assessed by the analysis of a certified reference material of milk (infant formula), and good agreement between the certified values and the measured value was obtained. The limits of quantification for the acid digestion with reflux system for Ca, Cu, Fe, K, and Na, in milligram per kilogram, were 7.48, 0.31, 1.0, 8.20, and 25.81, respectively, and for the microwave digestion were 14.0, 0.57, 1.78, 14.65, and 46.08, respectively. The decomposition procedure using a cold finger in an open system is effective, presenting the lowest residual carbon content (6 %), good accuracy, and relative standard deviation lower than 5 %, and appears to be a suitable procedure for sample preparation for routine analysis.

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Acknowledgments

The authors gratefully acknowledge the Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq), the Fundação de Amparo à Pesquisa do Estado de São Paulo, and CNPq/CAPES (Projeto Casadinho no. 552197/2011-4) for their financial support and scholarships.

Conflict of Interest

Eliézer Quadro Oreste has no conflict of interest. Alexander Ossanes de Souza has no conflict of interest. Camila Côrrea Pereira has no conflict of interest. Meibel Teixeira Lisboa has no conflict of interest. Mirla Janaína A. Cidade has no conflict of interest. Mariana Antunes Vieira has no conflict of interest. Solange Cadore has no conflict of interest. Anderson Schwingel Ribeiro has no conflict of interest.

Ethical Approval

This article does not contain any studies with human or animal subjects.

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Informed consent was obtained from all individual participants included in the study.

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Authors and Affiliations

  1. Laboratório de Metrologia Química (LabMeQui), Universidade Federal de Pelotas, 96160-000, Capão do Leão, RS, Brasil

    Eliézer Q. Oreste, Alexander O. de Souza, Camila C. Pereira, Meibel T. Lisboa, Mariana A. Vieira & Anderson S. Ribeiro

  2. Departamento de Química, Universidade Federal de Roraima, 69304-000, Boa Vista, RR, Brasil

    Mirla Janaína A. Cidade

  3. Institute of Chemistry, University of Campinas, P.O. Box 6154, 13083-970, Campinas, SP, Brasil

    Mirla Janaína A. Cidade & Solange Cadore

Authors
  1. Eliézer Q. Oreste
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  2. Alexander O. de Souza
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  3. Camila C. Pereira
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  4. Meibel T. Lisboa
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  5. Mirla Janaína A. Cidade
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  6. Mariana A. Vieira
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  7. Solange Cadore
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  8. Anderson S. Ribeiro
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Correspondence to Anderson S. Ribeiro.

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Oreste, E.Q., de Souza, A.O., Pereira, C.C. et al. Evaluation of Sample Preparation Methods for the Determination of Ca, Cu, Fe, K, and Na in Milk Powder Samples by ICP-OES. Food Anal. Methods 9, 777–784 (2016). https://doi.org/10.1007/s12161-015-0252-1

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  • DOI: https://doi.org/10.1007/s12161-015-0252-1

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