Determination of Trace Elements in Meat and Fish Samples by MIP OES Using Solid-Phase Extraction

  • 94 Accesses

  • 2 Citations


A new procedure for the determination of As, Cd, Cr, Cu, Hg, Pb, and Zn in fish and meat (bovine and ovine) samples by microwave-induced plasma optical emission spectrometry (MIP OES) was developed. The procedure is based on separation and preconcentration of analytes by solid-phase extraction (SPE), composed from the functionalization of silica with p-aminobenzoic acid (PABA-MCM-41). Factors that directly affect the SPE procedure as pH, buffer concentration, sample flow, and elution flow were evaluated through a factorial design (24). The optimized conditions employed at the proposed procedure were as follows: pH 9.5, 0.01 mol L−1 borate buffer concentration, sampling, and 6.0 mL min−1 of elution flow. Linear models were treated regarding the weighted regression, an optional strategy of the equipment, the weighted fit. The proposed procedure provides limits of quantification (LOQ) of 9.6, 2.8, 0.1, 0.2, 1.5, 13.3, and 3.9 μg g−1 for As, Cd, Cr, Cu, Hg, Pb, and Zn, respectively. Accuracy was assessed from the analysis of the certified reference materials (CRM) of dogfish liver (DOLT-5, NRC) and bovine liver (1577c, NIST), and a reference material of bovine liver (RM-Agro E3001a, EMBRAPA). The procedure was applied in local market meats (bovine and ovine) and fish (tilapia) samples, and it showed adequate for the determination of As, Cd, Cr, Cu, Hg, Pb, and Zn by MIP OES.

This is a preview of subscription content, log in to check access.

Access options

Buy single article

Instant unlimited access to the full article PDF.

US$ 39.95

Price includes VAT for USA

Subscribe to journal

Immediate online access to all issues from 2019. Subscription will auto renew annually.

US$ 99

This is the net price. Taxes to be calculated in checkout.

Fig. 1
Fig. 2
Fig. 3


  1. Agilent. Accessed on July 16, 2019

  2. Ahmad H, Jalil AA, Triwahyono S (2016) Dispersive solid phase extraction of gold with magnetite-graphene oxide prior to its determination: via microwave plasma-atomic emission spectrometry. RSC Adv 6:88110–88116.

  3. Ambushea A, Hlongwanea MM, McCrindlea Robert I, McCrindle Cheryl ME (2012) Assessment of levels of V, Cr, Mn, Sr, Cd, Pb and U in bovine meat. S Afr J Chem 65:159–164

  4. Amorim FAC, Costa VC, Guedes WN, Sa IP, Santos MC, Silva EGP, Lima DDC (2016) Multivariate optimization of method of slurry sampling for determination of iron and zinc in starch samples by flame atomic absorption spectrometry. Food Anal Methods 9:1719–1725.

  5. ANVISA (2013) National agency for sanitary surveillance - Resolução RDC n° 42 de 29 de agosto de 2013. Dispõe sobre o Regulamento Técnico MERCOSUL sobre Limites Máximos de Contaminantes Inorgânicos em Alimentos. Diário Oficial da União, Brasília, DF, Seção 1, 30 ago

  6. Ayala A, Takagai Y (2018a) Sequential injection analysis system exploiting on-line solid-phase extraction for the determination of strontium and nickel by microwave plasma atomic emission spectrometry. Anal Sci 34:387–390.

  7. Ayala A, Takagai Y (2018b) On-line pseudo-stationary magnetic solid-phase extraction using magnetic cation exchange microparticles and its application to the determination of strontium. J Anal At Spectrom 33:1251–1255.

  8. Batista ÉF, Pessoa AGG, Guerra MBB, Miranda K, Pereira-Filho ER (2012) Fast sequential determination of As and Sb, Bi and Pb by continuous flow hydride generation atomic absorption spectrometry. Food Anal Methods 6:1212–1222.

  9. Belitz HD, Grosch W, Schieberle P (2004) Food chemistry, 3rd edn. Springer, Berlin 1070 p

  10. Bezerra MA, Santos WNL, Korn M das GA, Ferreira SLC (2007) On-line system for preconcentration and determination of metals in vegetables by inductively coupled plasma optical emission spectrometry. J Hazard Mater 148:334–339.

  11. Bianchi SR, Peixoto AMJ, Souza JB, Tullio RR, Nogueira ARA (2016) Production and characterization of a bovine liver candidate reference material. J Phys Conf Ser 733:012006.

  12. Bosch A, O’Neill B, Sigge GO, Kerwath SE, Hoffmanb LC (2016) Heavy metals in marine fish meat and consumer health: a review. J Sci Food Agric 96:32–48.

  13. Calderilla C, Maya F, Leal L, Cerdà V (2018) Recent advances in flow-based automated solid-phase extraction. Trends Anal Chem 108:370–380.

  14. Chen X-L, Ai L-F, Cao Y-Q, Nian Q-X, Jia Y-Q, Hao Y-L, Wang M-M, Wang X-S (2019a) Rapid determination of sulfonamides in chicken muscle and milk using efficient graphene oxide-based monolith on-line solid-phase extraction coupled with liquid chromatography–tandem mass spectrometry. Food Anal Methods 12:271–281.

  15. Chen S, Yan J, Li J, Lu D (2019b) Dispersive micro-solid phase extraction using magnetic ZnFe2O4 nanotubes as adsorbent for preconcentration of Co(II), Ni(II), Mn(II) and Cd(II) followed by ICP-MS determination. Microchem J 147:232–238.

  16. Codex (2018) Committee on Contaminants in foods. General standards for contaminants and toxins in food and feed. CXS 193-1995

  17. Costa JAS, de Jesus RA, Dorst DD, Pinatti IM, Oliveira LMR, Mesquita ME, Paranhos CM (2017) Photoluminescent properties of the europium and terbium complexes covalently bonded to functionalized mesoporous material PABA-MCM-41. J Lumin 192:1149–1156.

  18. Daşbaşı T, Saçmacı Ş, Ülgen A, Kartal Ş (2016) Determination of some metal ions in various meat and baby food samples by atomic spectrometry. Food Chem 197:107–113.

  19. Evans EH, Horstwood M, Pisonero J, Smith CMM (2013) Atomic spectrometry update: review of advances in atomic spectrometry and related techniques. J Anal At Spectrom 28:779–800.

  20. Evans EH, Pisonero J, Smith CMM, Taylor RN (2015) Atomic spectrometry update: review of advances in atomic spectrometry and related techniques. J Anal At Spectrom 33:684–705.

  21. Feist B, Sitko R (2019) Fast and sensitive determination of heavy metal ions as batophenanthroline chelates in food and water samples after dispersive micro-solid phase extraction using graphene oxide as sorbent. Microchem J 147:30–36.

  22. Ferreira SLC (2015) Introdução às técnicas de planejamento de experimentos. Vento Leste, Salvador

  23. Ferreira SLC, Dos Santos WNL, Quintella CM, Neto BB, Bosque-Sendra JM (2004) Doehlert matrix: a chemometric tool for analytical chemistry—review. Talanta 63:1061–1067.

  24. Gallego Ríos SE, Peñuela GA, Ramírez Botero CM (2017) Method validation for the determination of mercury, cadmium, lead, arsenic, copper, iron, and zinc in fish through microwave-induced plasma optical emission spectrometry (MIP OES). Food Anal Methods 10:3407–3414.

  25. Gouda AA, Ghannam SMA (2016) Impregnated multiwalled carbon nanotubes as efficient sorbent for the solid phase extraction of trace amounts of heavy metal ions in food and water samples. Food Chem 202:409–416.

  26. Hu B, He M, Chen B (2015) Nanometer-sized materials for solid-phase extraction of trace elements. Anal Bioanal Chem 407:2685–2710.

  27. Khan M, Yilmaz E, Sevinc B, Sahmetlioglu E, Shah J, Jan MR, Soylak M (2016) Preparation and characterization of magnetic allylamine modified graphene oxide-poly(vinyl acetate-co-divinylbenzene) nanocomposite for vortex assisted magnetic solid phase extraction of some metal ions. Talanta 146:130–137.

  28. Korn M d GA, Morte ES d B, Santos DCMB, Castro JT, JTP B, Teixeira AP, Fernandes AP, Welz B, Santos WPC, Santos EBGN, Korn M (2008) Sample preparation for the determination of metals in food samples using spectroanalytical methods - a review. Appl Spectrosc Rev 43:67–92.

  29. Krug FJ, Rocha FRP (2019) Métodos de preparo de amostras. Fundamentos sobre o preparo de amostras orgânicas e inorgânicas para análise elementar, 2nd edn. Editora EditSBQ, São Paulo

  30. Liang G, Gong W, Li B, Li B, Zuo J, Pan L, Liu X (2019) Analysis of heavy metals in foodstuffs and an assessment of the health risks to the general public via consumption in Beijing, China. Int J Environ Res Public Health 16:909.

  31. Lima DC, Guedes WN, Costa VC, Amorin FAC (2018) Application of factorial design and desirability function to develop a single analytical procedure for the determination of metals in different tissues of blue crab (callinectes danac). J Braz Chem Soc 29:1885–1893.

  32. Machado RC, Amaral CDB, Nóbrega JA, Nogueira ARA (2017) Multielemental determination of As, Bi, Ge, Sb, and Sn in agricultural samples using hydride generation coupled to microwave-induced plasma optical emission spectrometry. J Agric Food Chem 65:4839–4842.

  33. Meira LA, Dias FS (2017) Application of constrained mixture design and Doehlert matrix in the optimization of dispersive liquid-liquid microextraction assisted by ultrasound for preconcentration and determination of cadmium in sediment and water samples by FAAS. Microchem J 130:56–63.

  34. Miller JN, Miller JC (2010) Statistics and chemometrics for analytical chemistry, 6th. Editora Pearson, England

  35. Oliveira AF, Gonzalez MH, Nogueira ARA (2018) Use of multiple lines for improving accuracy, minimizing systematic errors from spectral interferences, and reducing matrix effects in MIP OES measurements. Microchem J 143:326–330.

  36. Pereira F, Pereira-Filho E (2018) Aplicação De Programa Computacional Livre Em Planejamento De Experimentos: Um Tutorial. Quim Nova 2018:1061–1071.

  37. Pilarczyk R (2014) Concentrations of toxic and nutritional essential elements in meat from different beef breeds reared under intensive production systems. Biol Trace Elem Res 158:36–44.

  38. Rather IA, Koh WY, Paek WK, Lim J (2017) The sources of chemical contaminants in food and their health implications. Front Pharmacol 8.

  39. Sá IP, Santos LN, Silva EGP, Lima DC, Amorim FAC (2018) Preconcentration based on coprecipitation using silver chromate as a carrier for copper determination by FAAS. Quim Nova 42:10–16.

  40. Saha N, Mollah MZI, Alam MF, Safiur Rahman M (2016) Seasonal investigation of heavy metals in marine fishes captured from the Bay of Bengal and the implications for human health risk assessment. Food Control 70:110–118.

  41. Soylak M, Topalak Z (2014) Multiwalled carbon nanotube impregnated with tartrazine: solid phase extractant for Cd(II) and Pb(II). J Ind Eng Chem 20:581–585.

  42. Sun J, Liang Q, Han Q, Zhang X, Ding M (2015) One-step synthesis of magnetic graphene oxide nanocomposite and its application in magnetic solid phase extraction of heavy metal ions from biological samples. Talanta 132:557–563.

  43. Sun C, Zhang Y, Gong Z, Wang X, Yang Y, Wang Y (2018) Determination of trace elements in samples with high salt content by inductively coupled plasma mass spectrometry after solid-phase preconcentration. Int J Mass Spectrom 431:22–26.

  44. Thompson M, Ellison SLR, Wood R (2002) Harmonized guidelines for single laboratory. Pure Appl Chem 74:835–855.

  45. Vandeginste BGM, Massart DL, Buydens LMC, De Jong S, Lewi PJ, Smeyers-Verbeke J (1998) Handbook of chemometrics and qualimetrics: part a. Elsevier, Amsterdam

  46. Yavuz E, Senerife T, Sahan S (2013) FAAS determination of Ag(I) in water, anode slime, rock and cream samples by solid phase extraction method based on Sepabeads SP207/5. J Braz Chem Soc 24:736–742.

  47. Zhang J, Zhang G, Zhao C, Quan X, Jia Q (2012) On-line preconcentration/separation of inorganic arsenic and antimony by poly (aryl ether ketone) containing pendant carboxyl groups prior to microwave plasma atomic spectrometry determinations. Microchem J 100:95–99.

Download references

Author information

Correspondence to Ana Rita Araujo Nogueira.

Ethics declarations

This is an original research article that has neither been published previously or considered presently for publication elsewhere. All authors named in the manuscript are entitled to the authorship and have approved the final version of the submitted manuscript.

Conflict of Interest

Ivero Pita de Sá declares that he has no conflict of interest. Julymar Marcano Higuera declares that she has no conflict of interest. Vinicius Câmara Costa declares that he has no conflict of interest. José Arnaldo Santana Costa declares that he has no conflict of interest. Caio Marcio Paranhos da Silva declares that he has no conflict of interest, and Ana Rita Araujo Nogueira declares that she has no conflict of interest.

Ethical Approval

Not applicable.

Informed Consent

Informed consents were obtained from all individual participants included in the study.

Additional information

Publisher’s Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

de Sá, I.P., Higuera, J.M., Costa, V.C. et al. Determination of Trace Elements in Meat and Fish Samples by MIP OES Using Solid-Phase Extraction. Food Anal. Methods 13, 238–248 (2020) doi:10.1007/s12161-019-01615-3

Download citation


  • SPE
  • Factorial design
  • Fish
  • Meat
  • Trace elements