Food Analytical Methods

, Volume 8, Issue 1, pp 52–57 | Cite as

Analysis of Micronutrients and Heavy Metals in Portuguese Infant Milk Powders by Wavelength Dispersive X-ray Fluorescence Spectrometry (WDXRF)

  • Tânia A. P. Fernandes
  • José A. A. Brito
  • Luísa M. L. GonçalvesEmail author


Concentrations of trace mineral nutrients such as Cu, Fe, and Zn have been analyzed by WDXRF in eight different infant milk powders, representing the majority of the milk powder brands commercialized in Portuguese pharmacies. Results suggest that the concentrations of some of elements analyzed are not consistent with the values labeled by manufacturers. However, all fall inside the concentration ranges defined by the Portuguese and European legislations, except for Al. The presence of aluminum was detected in all analyzed formulations in an average concentration of 8.25 to 19.75 mg Kg−1. This study also reveals the feasibility of WDXRF for the quantitative analysis of trace mineral nutrients in milk powder samples. Moreover, the approach described herein, using the WDXRF technique in helium mode, presents a new methodological advantage over similar published studies. This technique may represent an option for quality control of milk powder formulations, particularly at their production site.


Infant milk powders Mineral nutrients Heavy metals WDXRF 



The authors wish to thank Egas Moniz Cooperativa de Ensino Superior, CRL, for the financial support.

Conflict of Interest

Tânia A. P. Fernandes declares that she has no conflict of interest. José A. Brito declares that he has no conflict of interest. Luísa L. Gonçalves declares that she has no conflict of interest. This article does not contain any studies with human or animal subjects.


  1. Abernethy DR, Destefano AJ, Cecil TL, Zaidi K, Williams RL (2010) Metal impurities in food and drugs. Pharm Res 27(5):750–755CrossRefGoogle Scholar
  2. Bruker (2004) Introduction to X-ray fluorescence analysis. Manual Bruker AXS GmbH, Karlsruhe, GermanyGoogle Scholar
  3. European Commission (2006) Commission Directive 2006/141/EC on infant formulae and follow-on formulae—Official Journal of the European Union, 401/1-401/33Google Scholar
  4. Gunicheva TN (2009) Advisability of X-ray fluorescence analysis of dry residue of cow milk applied to monitor environment. X- Ray Spectrometry 39(1):22–27CrossRefGoogle Scholar
  5. Hannan MA, Faraji B, Tanguma J, Longoria N, Rodriguez RC (2009) Maternal milk concentration of Zinc, Iron, Selenium, and Iodine and its relationship to dietary intakes. Biol Trace Elem Res 127(1):6–15CrossRefGoogle Scholar
  6. Ikem A, Nwankwoala A, Odueyungbo S, Nyavor K, Egiebor N (2002) Levels of 26 elements in infant formula from USA, UK, and Nigeria by microwave digestion and ICP-OES. Food Chem 77(4):439–447CrossRefGoogle Scholar
  7. International conference on harmonization of technical requirements for registration of pharmaceuticals for human use (ICH) (2005) Validation of analytical procedures: Text and Methodology Q2(R1, 1-13Google Scholar
  8. Kira CS, Maihara VA (2007) Determination of major and minor elements in dairy products through inductively coupled plasma optical emission spectrometry after wet partial digestion and neutron activation analysis. Food Chem 100(1):390–395CrossRefGoogle Scholar
  9. Korn MDGA, Morte ESB, Santos DCMB, Castro JC, Barbosa JTP, Teixeira AP, Fernandes AP, Welz B, Santos WPCS, Santos EBGN, Korn M (2008) Sample preparation for the determination of metals in food samples using spectroanalytical methods - A Review. Appl Spectrosc Rev 43(2):67–92CrossRefGoogle Scholar
  10. Lesniewicz A, Wroz A, Wojcik A, Zyrnicki W (2010) Mineral and nutritional analysis of Polish infant formulas. J Food Compos Anal 23(5):424–431CrossRefGoogle Scholar
  11. Lönnerdal B, Kelleher SL (2009) Micronutrient transfer: infant absorption. Adv Exp Med Biol 639:29–40CrossRefGoogle Scholar
  12. Marguí E, Fontàs C, Buendía A, Hidalgo M, Queralt I (2009) Determination of metal residues in active pharmaceutical ingredients according to European current legislation by using X-ray fluorescence spectrometry. J Anal At Spectrom 24(9):1253–1257CrossRefGoogle Scholar
  13. Navarro-Blasco I, Alvarez-Galindo JI (2003) Aluminium content of Spanish infant formula. Food Addit Contam 20(5):470–481CrossRefGoogle Scholar
  14. Nordberg GF, Fowler BA, Nordberg M (2007) Handbook on the toxicology of metals, 3rd ed. Academic Press, Maryland, USAGoogle Scholar
  15. Pashkova GV (2009) X-ray fluorescence determination of element contents in milk and dairy products. Food Anal Methods 2(4):303–310CrossRefGoogle Scholar
  16. Perring L, Andrey D (2003) EDXRF as a tool for rapid minerals control in milk-based products. J Agric Food Chem 51(15):4207–4212CrossRefGoogle Scholar
  17. Perring L, Andrey D (2004) Wavelength-dispersive X-ray fluorescence measurements on organic matrices: application to milk based products. X-Ray Spectroscopy 33(2):128–135CrossRefGoogle Scholar
  18. Perring L, Andrey D, Basic-Dvorzak M, Blanc J (2005a) a) Rapid multimineral determination in infant cereal matrices using wavelength dispersive X-ray fluorescence. J Agric Food Chem 53(12):4696–4700CrossRefGoogle Scholar
  19. Perring L, Andrey D, Basic-Dvorzak M, Hammer D (2005b) b) Rapid quantification of iron, copper and zinc in food premixes using energy dispersive X-ray fluorescence. J Food Compos Anal 18(7):655–663CrossRefGoogle Scholar
  20. Perring L, Blanc J (2008a) Faster measurement of minerals in milk powders: comparison of a high power wavelength dispersive XRF system with ICP-AES and potentiometry reference methods. Food Anal Methods 1(3):205–213CrossRefGoogle Scholar
  21. Perring L, Blanc J (2008b) Validation of quick measurement of mineral nutrients in milk powders: comparison of energy dispersive X-ray fluorescence with inductively coupled plasma-optical emission spectroscopy and potentiometry reference methods. Sens & Instrumen Food Qual 2(4):254–262CrossRefGoogle Scholar
  22. Saracoglu S, Saygu KO, Uluozlu OD, Tuzen M, Soylak M (2007) Determination of trace element contents of baby foods from Turkey. Food Chem 105(1):280–285CrossRefGoogle Scholar
  23. Rodriguez EM, Sanz AM, Díaz RC (2000) Concentrations of iron, copper and zinc in human milk and powdered infant formula. Int J Food Sci Nutr 51(5):373–380CrossRefGoogle Scholar
  24. Sola-Larrañaga C, Navarro-Blasco I (2009) Optimization of a slurry dispersion method for minerals and trace elements analysis in infant formulae by ICP-OES and FAAS. Food Chem 115(3):1048–1055CrossRefGoogle Scholar
  25. Tuzen M, Soylakb M (2007) Evaluation of trace elements in canned foods marketed from Turkey. Food Chem 102(4):1089–1095CrossRefGoogle Scholar
  26. Van Grieken RE, Markowicz AA (2002) Handbook of X-Ray spectrometry; methods and techniques, 2nd ed. Marcel Dekker, Inc, New York, USAGoogle Scholar
  27. Zand N, Chowdhry BZ, Zotor FB, Wray DS, Amuna P, Pullen FS (2011) Essential and trace elements content of commercial infant foods in the UK. Food Chem 128:123–128CrossRefGoogle Scholar
  28. World Health Organization/Food and Agriculture Organization of the United Nations (2007) Sixty-eighth report of the Joint FAO/WHO Expert Committee on Food Additives—evaluation of certain food additives and contaminants, WHO Technical Report Series (947)Google Scholar
  29. World Health Organization/Food and Agriculture Organization of the United Nations (2008) CAC/RCP 66-2008—Code of Hygienic Practice Powdered Formulae for Infants and Young Children, Codex Alimentarius Commission, 1-29Google Scholar

Copyright information

© Springer Science+Business Media New York 2014

Authors and Affiliations

  • Tânia A. P. Fernandes
    • 1
  • José A. A. Brito
    • 1
  • Luísa M. L. Gonçalves
    • 1
    Email author
  1. 1.Centro de Investigação Interdisciplinar Egas Moniz (CiiEM)Instituto Superior de Ciências da Saúde Egas Moniz, Campus UniversitárioCaparicaPortugal

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