Food Analytical Methods

, Volume 10, Issue 6, pp 1787–1799 | Cite as

Different Approaches for Digestion, Performance Assessment and Measurement Uncertainty for the Analysis of Cadmium and Lead in Feeds

  • Luciano Molognoni
  • Jaqueline Zarpelon
  • Leandro Antunes de Sá Ploêncio
  • Jacson Nascimento dos Santos
  • Heitor Daguer


Certain feedingstuffs are sources of contamination for animals with cadmium (Cd) and lead (Pb). Different approaches for sample digestion, performance assessment, and measurement uncertainty for the analysis of Pb and Cd by flame atomic absorption spectrometry were compared. Full method validation, including matrix effect and analytical limits, were assessed. Despite having a lower performance compared to the microwave digestion, dry ashing was a viable alternative for sample digestion, leading to lower operating costs. Interlaboratory validation proved to be a cheaper alternative, instead of the long traditional in-house approach. The method was suitable for routine analysis of several feed samples. There was a greater amount of quantifiable results for Pb, ranging from traces up to high concentrations (7430 ± 930 mg kg-1). Cd was also quantified in some samples, ranging from 0.11 ± 0.01 to 8.71 ± 0.90 mg kg−1. The higher concentrations of both metals were found in mineral mixtures and fish meal.


Dry digestion Microwave digestion Proficiency testing Top-down approach Traditional approach 



We acknowledge Food and Agriculture Organization of the United Nations and the Austrian Agency for Health and Food Safety for authorizing the use of the FAO-IAG Ringtests data. ICP-MS analyses were carried out at Universidade Federal de Santa Catarina. We would like to acknowledge Vera Lucia Azzolin Frescura Bascuñan for this facility. We are also grateful to Fundação de Amparo à Pesquisa e Inovação de Santa Catarina (FAPESC) for funding this research with fellowships (Grant No. 1683).

Compliance with Ethical Standards

Conflict of Interest

Luciano Molognoni declares that he has no conflict of interest. Jaqueline Zarpelon declares that she has no conflict of interest. Leandro Antunes de Sá Ploêncio declares that he has no conflict of interest. Jacson Nascimento dos Santos declares that he has no conflict of interest. Heitor Daguer declares that he has no conflict of interest.

Ethical Approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Informed Consent

Not applicable.


  1. Adeloju SB (1989) Comparison of some wet digestion and dry ashing methods for voltammetric trace element analysis. Analyst 455–461Google Scholar
  2. Akinyele IO, Shokunbi OS (2015) Comparative analysis of dry ashing and wet digestion methods for the determination of trace and heavy metals in food samples. Food Chem 173:682–684CrossRefGoogle Scholar
  3. Altundag H, Tuzen M (2011) Comparison of dry, wet and microwave digestion methods for the multi element determination in some dried fruit samples by ICP-OES. Food Chem Toxicol 49:2800–2807CrossRefGoogle Scholar
  4. Associação Brasileira de Normas Técnicas 2005. ABNT NBR ISO/IEC 17025: 2005. Requisitos gerais para a competência de laboratórios de ensaio e calibraçãoGoogle Scholar
  5. Aydin I (2008) Comparison of dry, wet and microwave digestion procedures for the determination of chemical elements in wool samples in Turkey using ICP-OES technique. Microchem J 90:82–87CrossRefGoogle Scholar
  6. Borges SS, Beinner MA, Silva JBB (2015) Direct method for determination of Al, Cd, Cu, and Pb in beers in situ digested by GF AAS using permanent modifiers. Biol Trace Elem Res 167:155–163CrossRefGoogle Scholar
  7. Brasil, Ministério da Agricultura, Pecuária e Abastecimento (MAPA) 2011. Guia de validação e controle da qualidade analítica: Fármacos em produtos para alimentação animal e medicamentos veterinários, Secretaria de defesa agropecuária. MAPA/ACS, BrasíliaGoogle Scholar
  8. Codex Alimentarius Commission 2011. CAC/GL 54–2004. Guidelines on measurement uncertainty, rev. 1, RomeGoogle Scholar
  9. Coelho I, Gueifão S, Matos AS, Roe M, Castanheira I (2013) Experimental approaches for the estimation of uncertainty in analysis of trace inorganic contaminants in foodstuffs by ICP-MS. Food Chem 141:604–611CrossRefGoogle Scholar
  10. Demirel S, Tuzen M, Saracoglu S, Soylak M (2008) Evaluation of various digestion procedures for trace element contents of some food materials. J Hazard Mater 152:1020–1026CrossRefGoogle Scholar
  11. Duffus JH (2002) “Heavy metals”—a meaningless term? Pure Appl Chem 74:793–807CrossRefGoogle Scholar
  12. Durduran E, Altundag H, Imamoglu M, Yıldız SZ, Tuzen M (2015) Simultaneous ICP-OES determination of trace metals in water and food samples after their preconcentration on silica gel functionalized with N-(2-aminoethyl)-2, 3-dihydroxybenzaldimine. J Ind Eng Chem 27:245–250CrossRefGoogle Scholar
  13. EFSA (2004) Opinion of the scientific panel on contaminants in the food chain on a request from the commission related to Cd as undesirable substance in animal feed. The EFSA Journal 72:1–24Google Scholar
  14. EFSA (2009) Scientific opinion of the panel on contaminants in the food chain on a request from the European Commission on Cd in food. The EFSA Journal 980:1–139Google Scholar
  15. Ellison SL (2014) Implementing measurement uncertainty for analytical chemistry: the Eurachem guide for measurement uncertainty. Metrologia 51:S199CrossRefGoogle Scholar
  16. Enders A, Lehmann J (2012) Comparison of wet-digestion and dry-ashing methods for total elemental analysis of biochar. Commun Soil Sci Plant Anal 43:1042–1052CrossRefGoogle Scholar
  17. Eurolab (2007). Technical Report No. 1/2007. Measurement uncertainty revisited: alternative approaches to uncertainty evaluationGoogle Scholar
  18. European Commission 2002a. Directive 2002/32/EC. Undesirable substances in animal feed. Directive of the European Parliament and of the Council of 7 May 2002 on 2002/32Google Scholar
  19. European Commission 2002b. Commission decision 2002/657/EC of 12 August 2002. Implementing council directive 96/23/EC concerning performance of analytical methods and the interpretation of results. Off J Eur Communities. L 2221/8Google Scholar
  20. Gonçalves MLSS (1983) Métodos Instrumentais para Análise de Soluções—Análise Quantitativa. Fundação Calouste-Gulbenkian, LisboaGoogle Scholar
  21. Granato D, Calado VMA, Jarvis B (2014) Observations on the use of statistical methods in food science and technology. Food Res Int 55:137–149CrossRefGoogle Scholar
  22. ISO/IEC Guide 98-3:2008 2008, Uncertainty of measurement—part 3: guide to the expression of uncertainty in measurement (GUM:1995), International Organization for Standardization, Geneve, SwitzerlandGoogle Scholar
  23. Lecomte F, Hubert C, Demarche S, De Bleye C, Dispas A, Jost M, Frankenne F, Ceccato A, Rozet E, Hubert P (2012) Comparison of the quantitative performances and measurement uncertainty estimates obtained during method validation versus routine applications of a novel hydrophilic interaction chromatography method for the determination of cidofovir in human plasma. J Pharm Biomed Anal 57:153–165CrossRefGoogle Scholar
  24. López-Alonso M, Fink-Gremmels J (2012) Animal feed contamination by toxic metals. In: Animal feed contamination, effects on livestock and food safety. Woodhead Publishing, Cambridge, pp. 183–201CrossRefGoogle Scholar
  25. Lucatello L, Cagnardi P, Capolongo F, Ferraresi C, Bernardi F, Montesissa C (2015) Development and validation of an LC–MS/MS/MS method for the quantification of fluoroquinolones in several matrices from treated turkeys. Food Control 48:2–11CrossRefGoogle Scholar
  26. MacCarthy HT, Ellis PC (1990) Comparison of microwave digestion with conventional wet ashing and dry ashing digestion for analysis of Pb, Cd, chromium, copper, and zinc in shellfish by flame atomic absorption spectroscopy. Journal-Association of Official Analytical Chemists 74:566–569Google Scholar
  27. MacDonald M, Mannion C, Rafter PA (2009) Confirmatory method for the simultaneous extraction, separation, identification and quantification of tetracycline, sulphonamide, trimethoprim and dapsone residues in muscle by ultra-high performance liquid chromatography–tandem mass spectrometry according to commission decision 2002/657/EC. J Chromatogr A 1216:8110–8116CrossRefGoogle Scholar
  28. Magnusson B, Näykki T, Hovind H, Krysell M (2004) Handbook for calculation of measurement uncertainty in environmental laboratories. Nordtest Report TR, 537Google Scholar
  29. Medina-Pastor P, Valverde A, Pihlström T, Masselter S, Gamon M, Mezcua M, Rodriguez-Torreblanca C, Fernández-Alba AR (2011) Comparative study of the main top-down approaches for the estimation of measurement uncertainty in multiresidue analysis of pesticides in fruits and vegetables. J Agric Food Chem 59:7609–7619CrossRefGoogle Scholar
  30. Molognoni L, Vitali L, Ploêncio LAS, Santos JN, Daguer H (2016) Determining the arsenic, Cd, Pb, copper and chromium contents by atomic absorption spectrometry in Pangasius fillets from Vietnam. J Sci Food Agric 96:3109–3113CrossRefGoogle Scholar
  31. Rozet E, Rudaz S, Marini RD, Ziémons E, Boulanger B, Hubert P (2011) Models to estimate overall analytical measurements uncertainty: assumptions, comparisons and applications. Anal Chim Acta 702:160–171CrossRefGoogle Scholar
  32. Thompson M, Ellison SLR, Wood R (2006) The international harmonized protocol for the proficiency testing of analytical chemistry laboratories (IUPAC technical report). Pure Appl Chem 78:105–196CrossRefGoogle Scholar
  33. Vassileva E, Hoenig M (2011) Determination of the total and extractable mass fractions of Cd and Pb in mineral feed by using isotope dilution inductively coupled plasma mass spectrometry. Anal Chim Acta 701:37–44CrossRefGoogle Scholar
  34. Waalkes MP (2000) Cd carcinogenesis in review. J Inorg Biochem 79:241–244CrossRefGoogle Scholar
  35. WHO Library Cataloguing in Publication Data 2010. Evaluation of certain food additives and contaminants: seventy-third report of the Joint FAO/WHO Committee on food additives. 73rd: Geneva, Switzerland. IV.SeriesGoogle Scholar
  36. Yang L, Li Y, Ma X, Yan Q (2013) Comparison of dry ashing, wet ashing and microwave digestion for determination of trace elements in periostracum serpentis and periostracum cicadae by ICP-AES. J Chil Chem Soc 58:1876–1879CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2016

Authors and Affiliations

  1. 1.Ministério da Agricultura, Pecuária e AbastecimentoLaboratório Nacional Agropecuário (SLAV/LANAGRO/RS)Rua João Grumiché, 117, São JoséBrazil
  2. 2.Instituto Catarinense de Sanidade Agropecuária (ICASA)FlorianópolisBrazil
  3. 3.Universidade Federal de Santa CatarinaFlorianópolisBrazil

Personalised recommendations