A Green Analytical Method for the Multielemental Determination of Halogens and Sulfur in Pet Food

  • Julia Eisenhardt de Mello
  • Diogo La Rosa Novo
  • Gilberto Silva Coelho Junior
  • Priscila Tessmer Scaglioni
  • Marcia Foster MeskoEmail author


A suitable and green analytical method using microwave-induced combustion and ion chromatography with conductivity detection (IC-CD) and mass spectrometry detection (IC-MS) was proposed for the halogens and sulfur determination in pet food using a single analysis. Samples (up to 500 mg) were efficiently digested in a closed system under oxygen pressure (20 bar). Ultrapure water and 50 mmol L−1 or 100 mmol L−1 (NH4)2CO3 were evaluated as absorbing solutions. Trueness was evaluated by recovery tests using standard solution and certified reference materials. In both tests, mean recoveries ranging from 91 to 108% for all analytes were obtained using 50 mmol L−1 (NH4)2CO3 as absorbing solution. AOAC International recommended official methods for Cl and F determination in animal feed were also performed. Results for Cl using proposed method were in agreement with those obtained using AOAC official method, while the results for F were not compared between them because the concentration in the samples using AOAC official method was not detected. Precision was evaluated in terms of repeatability and the relative standard deviations (RSDs) using the proposed method were always lower than 8%. The proposed method presents several advantages when compared with AOAC International official methods such as the multielemental determination capability, lower waste generation, lower limits of detection, lower RSDs, and higher sample throughput. Sixteen samples destined to cats or dogs from different manufacturers were analyzed and the results showed a wide variation. These results indicate that an efficient quality control should be performed, and the proposed method is an excellent alternative as a new analytical tool for routine analysis of pet food.


Pet food analysis Food safety Halogens determination Microwave-induced combustion Ion chromatography Mass spectrometry 


Funding Information

The authors are grateful to Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES-Brazil) finance code 001, Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq-Brazil) grant numbers 409357/2016-2 and 309424/2016-0, and Fundação de Amparo à Pesquisa do Estado do Rio Grande do Sul (FAPERGS-Brazil) grant number 16/2551-0000561-8, for supporting this study.

Compliance with Ethical Standards

Conflict of Interest

Julia Eisenhardt de Mello declares that she has no conflict of interest. Diogo La Rosa Novo declares that he has no conflict of interest. Gilberto Silva Coelho Junior declares that he has no conflict of interest. Priscila Tessmer Scaglioni declares that she has no conflict of interest. Marcia Foster Mesko declares that she 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. AAFCO - Association of American Feed Control Officials (2016) Dog and cat food nutrient profiles. Official publication. Accessed 17 Feb 2019
  2. Barbosa JTP, Santos CMM, Bispo LS, Lyra FH, David JM, Korn MGA, Flores EMM (2013) Bromine, chlorine, and iodine determination in soybean and its products by ICP-MS after digestion using microwave-induced combustion. Food Anal Methods 6:1065–1070. CrossRefGoogle Scholar
  3. Brown D (2014) Bromine reference module in biomedical sciences - encyclopedia of toxicology, 3rd edn, pp 557–558Google Scholar
  4. Coelho GS Jr, Pereira RM, Hartwig CA, Toralles IG, Pereira CMP, Costa VC, Mesko MF (2017) Determination of Cl and S in edible seaweed by ion chromatography after decomposition by microwave-induced combustion. RVq 9:492–501. Google Scholar
  5. Costa SSL, Pereira ACL, Passos EA, Alves JPH, Garcia CAB, Araujo RGO (2013) Multivariate optimization of an analytical method for the analysis of dog and cat foods by ICP OES. Talanta 108:157–164. CrossRefGoogle Scholar
  6. Costa VC, Picoloto RS, Hartwig CA, Mello PA, Flores EMM, Mesko MF (2015) Feasibility of ultra-trace determination of bromine and iodine in honey by ICP-MS using high sample mass in microwave-assisted combustion. Anal Bioanal Chem 407:7957–7964. CrossRefGoogle Scholar
  7. Crizel MG, Hartwig CA, Novo DLR, Toralles IG, Schmidt L, Muller EI, Mesko MF (2015) A new method for chlorine determination in commercial pet food after decomposition by microwave-induced combustion. Anal Methods 7:4315–4320. CrossRefGoogle Scholar
  8. Dibartola SP (1992) Fluid therapy in small animal practice, 2nd edn. W.B. Saunders company, PhiladelphiaGoogle Scholar
  9. Duran A, Tuzen M, Soylak M (2010) Trace element concentrations of some pet foods commercially available in Turkey. Food Chem Toxicol 48:2833–2837. CrossRefGoogle Scholar
  10. Everett ET (2011) Fluoride’s effects on the formation of teeth and bones, and the influence of genetics. J Dent Res 90(5):552–560. CrossRefGoogle Scholar
  11. Flores EMM, Barin JS, Mesko MF, Knapp G (2007) Sample preparation techniques based on combustion reactions in closed vessels – a brief overview and recent applications. Spectrochim Acta B 62:1051–1064. CrossRefGoogle Scholar
  12. Hartwig CA, Toralles IG, Crizel MG, Müller ALH, Picoloto RS, Flores EMM, Mesko MF (2014) Determination of bromine and iodine in shrimp and its parts by ICP-MS after decomposition using microwave-induced combustion. Anal Methods 6:7540–7546. CrossRefGoogle Scholar
  13. Horwitz W, Latimer GW (2011) Official methods of analysis of Association of Official Analytical Chemists (AOAC) international, 18th edn, GaithersburgGoogle Scholar
  14. IUPAC. Compendium of Chemical Terminology (1997) McNaught, AD, Wilkinson A, 2nd ed., Blackwell Scientific Publications, OxfordGoogle Scholar
  15. Kapp RW Jr (2014) Fluorine. Reference module in biomedical sciences - encyclopedia of toxicology, 3rd edn, pp 611–615Google Scholar
  16. Mccall AS, Cummings CF, Bhave G, Vanacore R, Page-Mccaw A, Hudson BG (2014) Bromine is an essential trace element for assembly of collagen IV scaffolds in tissue development and architecture. Cell 157:1380–1139. CrossRefGoogle Scholar
  17. McKenzie RA, Carmichael AM, Schibrowski ML, Duigan SA, Gibson JA, Taylor JD (2009) Sulfur-associated polioencephalomalacia in cattle grazing plants in the family Brassicaceae. Aust Vet J 87:27–32. CrossRefGoogle Scholar
  18. Mesko MF, Pereira RM, Scaglioni PT, Novo DLR (2019) Single analysis of human hair for determining halogens and sulfur after sample preparation based on combustion reaction. Anal Bioanal Chem Accepted.
  19. Novo DLR, Pereira RM, Costa VC, Hartwig CA, Mesko MF (2018) A novel and eco-friendly analytical method for phosphorus and sulfur determination in animal feed. Food Chem 246:422–427. CrossRefGoogle Scholar
  20. Pereira JSF, Mello PA, Moraes DP, Duarte FA, Dressler VL, Knapp G, Flores EMM (2009) Chloride and sulfur determination in extra-heavy crude oil by inductively coupled plasma optical emission spectrometry after microwave-induced combustion. Spectrochim Acta B 64:554–558. CrossRefGoogle Scholar
  21. Perring L, Nicolas M, Andrey D, Rime CF, Richoz-Payot J, Dubascoux S, Poitevin E (2017) Development and validation of an ED-XRF method for the fast quantification of mineral elements in dry pet food samples. Food Anal Methods 10:1469–1478. CrossRefGoogle Scholar
  22. Rondan FS, Hartwig CA, Novo DLR, Moraes DP, Cruz SM, Mello PA, Mesko MF (2018) Ultra-trace determination of bromine and iodine in rice by ICP-MS after microwave-induced combustion. J Food Compos Anal 66:199–204. CrossRefGoogle Scholar
  23. Silva JS, Diehl LO, Frohlich AC, Costa VC, Mesko MF, Duarte FA, Flores EMM (2017) Determination of bromine and iodine in edible flours by inductively coupled plasma mass spectrometry after microwave-induced combustion. Microchem J 133:246–250. CrossRefGoogle Scholar
  24. Taflik T, Duarte FA, Flores ELM, Antes FG, Paniz JNG, Flores EMM, Dressler VL (2012) Determination of bromine, fluorine and iodine in mineral supplements using pyrohydrolysis for sample preparation. J Braz Chem Soc 23:488–495. CrossRefGoogle Scholar
  25. Todorov TI, Smith T, Abdalla A, Mapulanga S, Homes P, Hamilton M, Lewis T, McDonald M (2018) Comparison of ICP-MS and spectrophotometry methods for the analysis of iodine in 2013 US FDA total diet study samples. Food Anal Methods 11:3211–3223. CrossRefGoogle Scholar
  26. WHO – World Health Organization (2007) Assessment of iodine deficiency disorders and monitoring their elimination - a guide for programme managers. World Health Organization, GenevaGoogle Scholar
  27. Zhong Z, Li G, Zhu B, Luo Z, Huang L, Wu X (2012) A rapid distillation method coupled with ion chromatography for the determination of total sulphur dioxide in foods. Food Chem 131:1044–1050. CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC, part of Springer Nature 2019

Authors and Affiliations

  1. 1.Centro de Ciências Químicas, Farmacêuticas e de AlimentosUniversidade Federal de PelotasCapão do LeãoBrazil

Personalised recommendations