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Food Analytical Methods

, Volume 10, Issue 6, pp 1631–1644 | Cite as

A Rapid Single-Extraction Method for the Simultaneous Determination of Aflatoxins B1, B2, G1, G2, Fumonisin B1, and Zearalenone in Corn Meal by Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

  • Fabiano Narciso Paschoal
  • Daniela de Azevedo Silva
  • Rafael von Sperling de Souza
  • Marize Silva de Oliveira
  • Danilo Augusto Alves Pereira
  • Scheilla Vitorino Carvalho de Souza
Article

Abstract

A single-extraction method to simultaneously determine aflatoxins (B1, B2, G1, G2), fumonisin B1, and zearalenone in corn meal by ultra performance liquid chromatography tandem mass spectrometry, using a triple quadrupole, was optimized, validated, and applied in an occurrence study. Different extraction solutions were tested, with better performance for methanol/acetonitrile/water (60:20:20, v/v/v). Linearity was observed from 0.25 to 1.50 ng/mL for aflatoxins, from 20 to 120 ng/mL for fumonisin, and from 7.00 to 42.00 ng/mL for zearalenone. Significant matrix effects were shown for all groups. Selectivity was demonstrated, as matrix or spectral interferences were not observed at the predicted retention time window of the target analytes. Average recoveries of 87.57, 93.18, 93.35, 94.20, 78.76, and 95.98% were obtained for aflatoxins (B1, B2, G1, and G2) fumonisin and zearalenone, respectively. A z-score of 0.19 was estimated in a corn certified reference material for fumonisin B1. Maximum relative standard deviation values under repeatability and intermediate precision conditions were determined to be 13.6 and 13.6% for aflatoxins, 3.7 and 6.3% for fumonisin, and 3.5 and 4.0% for zearalenone, respectively. In the occurrence study, 50 samples were analyzed and 44% had measurable levels of fumonisin. Zearalenone was detected in 18%. The proposed method showed considerable advantages, considering environmental impacts, efficiency, and reliability.

Keywords

Mycotoxins Food Mass spectrometry Multigroup determination Single-laboratory validation Application 

Notes

Acknowledgments

The authors acknowledge the friends at the Mycotoxins Laboratory of the Ezequiel Dias Foundation and those at the Food Science Laboratory of the Federal University of Minas Gerais. We would also like to thank Waters Technologies in Brazil for their technical support and FAPEMIG for the financial support.

Compliance with Ethical Standards

Conflict of Interest

Fabiano Narciso Paschoal declares that he has no conflict of interest. Daniela de Azevedo Silva declares that she has no conflict of interest. Rafael von Sperling de Souza declares that he has no conflict of interest. Marize Silva de Oliveira declares that she has no conflict of interest. Danilo Augusto Alves Pereira declares that he has no conflict of interest. Scheilla Vitorino Carvalho de Souza 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.

References

  1. ABIMILHO (2011) Associação Brasileira das Indústrias de Milho. [Online] Available at: http://www.abimilho.com.br/milho/cereal. Accessed 02 Setembro 2013
  2. ABNT (2002) Associação Brasileira de Normas Técnicas—ABNT. ABNT ISO GUIA 33:2002. Utilização de materiais de referência certificados. In: Rio de Janeiro (ed) p 28Google Scholar
  3. AOAC (2016) Official Methods of Analysis of AOAC International. 20th, Cap. 49 ed. MarylandGoogle Scholar
  4. Arroyo-Manzanares N, Huertas-Pérez JF, Gámiz-Gracia L, García-Campaña AM (2013) A new approach in sample treatment combined with UHPLC-MS/MS for the determination of multiclass mycotoxins in edible nuts and seeds. Talanta 115:61–67CrossRefGoogle Scholar
  5. Beltrán E et al (2013) Development of sensitive and rapid analytical methodology for food analysis of 18 mycotoxins included in a total diet study. Anal Chim Acta 783:39–48CrossRefGoogle Scholar
  6. Berthiller F, Schuhmacher R, Buttinger G, Krska R (2005) Rapid simultaneous determination of major type A- and B-trichothecenes as well as zearalenone in maize by high performance liquid chromatography-tandem mass spectrometry. J Chromatogr 1062:209–216CrossRefGoogle Scholar
  7. Bertuzzi T, Rastelli S, Mulazzi A, Pietri A (2012) Evaluation and improvement of extraction methods for the analysis of aflatoxins B1, B2, G1 and G2 from naturally contaminated maize. Food Anal Methods 5:512–519CrossRefGoogle Scholar
  8. Burke S (2001) Regression and calibration. LC GC Europe Online Supplement, Buckinghamshire, pp 13–18Google Scholar
  9. Capriotti AL et al (2012) Multiclass mycotoxin analysis in aood, environmental and biological matrices with chromatography/mass spectrometry. Mass Spectrom Rev 31:466–503CrossRefGoogle Scholar
  10. Cavaliere C et al (2005) Development of a multiresidue method for analysis of major fusarium mycotoxins in corn meal using liquid chromatography/tandem mass spectrometry. Rapid Commun Mass Spectrom 19:2085–2093CrossRefGoogle Scholar
  11. Cifuentes A (2012) Food analysis: present, future and foodomics. Anal Chem 2012:1–16Google Scholar
  12. Dall’Asta C et al (2009a) Difficulties in fumonisin determination: the issue of hidden fumonisins. Anal Bioanal Chem 395:1335–1345CrossRefGoogle Scholar
  13. Dall’Asta C et al (2009b) Free and bound fumonisins in gluten-free food. Molecular Nutritional Food Research 53:492–499CrossRefGoogle Scholar
  14. EC (2002) Implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. s.l.:Official Journal of the European Communities L 221/8-L221/36Google Scholar
  15. EC (2006) Commission Regulation (EC) N° 401/2006 Laying down the methods of sampling and analysis for the official control of the levels of mycotoxins in foodstuffs. s.l.:Official Journal of the European Union L 70/12-L70/34Google Scholar
  16. Faberi A et al (2005) Determination of type B fumonisins mycotoxins in maize and maize-based products by liquid chromatography/tandem mass spectrometry using QqQ linear ion trap mass spectrometer. Rapid Commun Mass Spectrom 19:275–282CrossRefGoogle Scholar
  17. Frenich AG, Vidal JL, Romero-Gonzalez R, Aguilera-Luiz MDM (2009) Simple and high-throughput method for the multimycotoxin analysis in cereals and related foods by ultra high performance liquid chromatography / tandem mass spectrometry. Food Chem 117:705–712CrossRefGoogle Scholar
  18. Frenich AG, Romero-González R, del Mar Aguilera-Luiz M (2014) Comprehensive analysis of toxics (pesticides, veterinary drugs and mycotoxins) in food by UHPLC-MS. Trends Anal Chem 63:158–169CrossRefGoogle Scholar
  19. Generotti S, Cirlini M, Dall’Asta C, Suman M (2015) Influence of the industrial process from caryopsis to cornmeal semolina on levels of fumonisins and their masked forms. Food Control 48:170–174Google Scholar
  20. Horwitz W (1982) Evaluation of analytical methods used for regulation of food and drugs. Anal Chem 54:67A–76ACrossRefGoogle Scholar
  21. Lattanzio V, Solfrizzo M, Powers S, Visconti A (2007) Simultaneous determination of aflatoxins, ochratoxin A and fusarium toxins in maize by liquid chromatography/tandem mass spectrometry after multitoxin immunoaffinity cleanup. Rapid Commun Mass Spectrom 21:3253–3261CrossRefGoogle Scholar
  22. Lattanzio VMT, Della Gatta S, Suman M, Visconti A (2011) Development and in-house validation of a robust and sensitive solid-phase extraction liquid chromatography/tandem mass spectrometry method for the quantitative determination of aflatoxins B1, B2 G1, G2, ocra, don, zon, T-2 e HT-2 in cereal-based foods. Rapid Communication in Mass Spectrometry 25:1869–1880CrossRefGoogle Scholar
  23. Li W, Herrman TJ, Dai SY (2010) Rapid determination of fumonisins in corn-based products by liquid chromatography / tandem mass spectrometry. Food Chemical Contaminants 93:1472–1481Google Scholar
  24. Malik AK, Kumar A et al (2010) Liquid chromatography-mass spectrometry in food safety. J Chromatogr A 1217(25):4018–4040CrossRefGoogle Scholar
  25. Oplatowska-Stachowiak M et al (2015) Determination of the mycotoxin content in distiller’s dried grain with solubles using a multianalyte UHPLC–MS/MS method. J Agric Food Chem 63:9441–9451CrossRefGoogle Scholar
  26. Oueslati S, Romero-González R, Lasram S, Frenich AG, Vidal JLM (2012) Multi-mycotoxin determination in cereals and derived products marketed in Tunisia using ultra-high performance liquid chromatography coupled to triple quadrupole mass spectrometry. Food Chem Toxicol 50:2376–2381CrossRefGoogle Scholar
  27. Paes MCD (2006) Aspectos físicos, Químicos e tecnológicos do Grão de Milho. Embrapa Milho e Sorgo, Sete Lagoas, MGGoogle Scholar
  28. Picó Y (2016) Mycotoxins: occurrence and determination. Reference Module in Food Science. In: Caballero B, Finglas P, Toldrá F (eds) Encyclopedia of Food and Health, 1st edn. Elsevier, Oxford, pp 35–42Google Scholar
  29. Ren Y et al (2011) Simultaneous determination of fomonisins B1, B2 and B3 contaminants in maize by ultra high-performance liquid chromatography tandem mass spectrometry. Anal Chim Acta 692:138–145CrossRefGoogle Scholar
  30. Resanovic RD et al (2013) Mycotoxins and their effect on human health. J Nat Sci Res 124:315–324Google Scholar
  31. Rychlik M et al (2014) Proposal of a comprehensive definition of modified and other forms of mycotoxins including “masked” mycotoxins. Mycotoxin Research 30:197–205CrossRefGoogle Scholar
  32. Senyuva HZ, Gilbert J, Stroka J (2010) Determination of fumonisins B1 and B2 in corn by LC/MS with immunoaffinity column cleanup: interlaboratory study. Food Chemical Contaminants 93(2):611–621Google Scholar
  33. Soleimany F, Jinap S, Abas F (2012) Determination of mycotoxins en cereals by liquid chromatography tandem mass spectrometry. Food Chem 130:1055–1060CrossRefGoogle Scholar
  34. Souza SVC, Junqueira RG (2005) A procedure to assess linearity by ordinary least squares method. Analitica Chimica Acta 552:25–35CrossRefGoogle Scholar
  35. Souza S, Pinto C, Junqueira R (2007) In-house method validation: application in arsenic analysis. J Food Compos Anal 20:241–247CrossRefGoogle Scholar
  36. Spanjer MC, Rensen PM, Scholten JM (2007) LC-MS/MS multi-method for mycotoxins after single extraction, with validation data for peanut, pistachio, wheat, maize, raisins and figs. Food Additives & Contaminants 25:1–18Google Scholar
  37. Stroka J, Petz M, Joerissen U, Anklam E (1999) Investigation of various extractants for the analysis of aflatoxin B1 in different food and feed matrices. Food Additives & Contaminants 16:331–338CrossRefGoogle Scholar
  38. Sulyok M, Berthiller F, Krska R, Schuhmacher R (2006) Development and validation of a liquid chromatography/tandem mass spectrometry method for the determination of 39 mycotoxins en wheat and maize. Rapid Commun Mass Spectrom 20:2649–2659CrossRefGoogle Scholar
  39. Tanaka H et al (2010) Determination of fusarium mycotoxins by liquid chromatography / tandem mass spectrometry coupled with immunoaffinity extraction. Rapid Commun Mass Spectrom 24:2445–2452CrossRefGoogle Scholar
  40. Thompson M (2000) Recent trends in inter-laboratory precision at ppb and sub-ppb concentrations in relation to fitness for purpose criteria in proficiency testing. Analyst 125:385–386CrossRefGoogle Scholar
  41. Thompson M, Ellison SLR, Wood R (2002) Harmonized guidelines for single-laboratory validation of methods of analysis. Pure Appl Chem 74:835–855CrossRefGoogle Scholar
  42. USDA (2015) Production, supply and distribution [Online]. Available at: http://www.fas.usda.gov/psdonline/psdQuery.aspx. Accessed 6 Jan 2015
  43. Varga E et al (2012) Stable isotope dilution assay for the accurate determination of mycotoxins in maize by HPLC-MS/MS. Analytical Bioanalytical Chemistry 402:2675–2686CrossRefGoogle Scholar
  44. Varga E, Glauner T, Berthiller F, Krska R, Schuhmacher R, Sulyok M (2013) Development and validation of a (semi-)quantitative UHPLC-MS/MS method for the determination of 191 mycotoxins and other fungal metabolites in almonds, hazelnuts, peanuts and pistachios. Anal Bioanal Chem 405:5087–5104CrossRefGoogle Scholar
  45. Visconti A, Solfrizzo M, De Girolamo A (2001) Determination of fumonisins B1 and B2 in cornflakes by high performance liquid chromatography and immunoaffinity clean-up. Food Additives & Contaminants 18:227–235CrossRefGoogle Scholar
  46. Zachariasova M et al (2010) Novel aproach in analysis of fusarium mycotoxins in cereals employing ultra performance liquid chromatography coupled with high resolution mass spectrometry. Anal Chim Acta 662:51–51CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2016

Authors and Affiliations

  • Fabiano Narciso Paschoal
    • 1
    • 2
  • Daniela de Azevedo Silva
    • 2
  • Rafael von Sperling de Souza
    • 2
  • Marize Silva de Oliveira
    • 2
  • Danilo Augusto Alves Pereira
    • 3
  • Scheilla Vitorino Carvalho de Souza
    • 1
  1. 1.Department of Food Science, Faculty of Pharmacy (FAFAR)Federal University of Minas Gerais (UFMG)Belo HorizonteBrazil
  2. 2.Mycotoxins LaboratoryEzequiel Dias FoundationBelo HorizonteBrazil
  3. 3.Waters Technology-BrazilAlameda TocantinsBarueriBrazil

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