Abstract
A fast, easy, and cheap method for the simultaneous determination and quantification of aflatoxins (B1, B2, G1, G2), T-2 and HT-2 toxins, and fumonisins (B1, B2) in cereal-derived products was developed. This method involved a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction coupled with liquid chromatography-tandem mass spectrometry. The method validation was performed by analyzing samples spiked at four levels, and the recoveries ranged from 83.6 to 102.9%, whereas the maximum values of repeatability and within-laboratory reproducibility were 14.3 and 15.7% following the performance criteria set by the European legislation. The method was then applied for the analysis of 21 cereal-derived products purchased on the Italian market, which were correctly packaged and labeled as intended for human consumption. The co-occurrence of more than one mycotoxin in the analyzed samples could represent a risk for consumers, and the described method could be a valid alternative for their simultaneous detection in the framework of official control.
Similar content being viewed by others
References
Reyneri A. The role of climatic condition on micotoxin production in cereal. Vet Res Commun. 2006;30:87–92.
European Food Safety Authority. Opinion of the scientific panel on contaminants in food chain on a request from the Commission related to fumonisins as undesirable substances in animal feed. The EFSA J. 2005;235:1–32.
International Agency for Research on Cancer. Summaries and evaluations: fumonisin B1. Lyon, France; 2002a. pp. 1–301.
Yang S, Wang Y, Beier RC, Zhang H, De Ruyck K, Sun F, et al. Simultaneous determination of type A and B trichothecenes and their main metabolites in food animal tissues by ultra-performance liquid chromatography coupled with triple quadrupole mass spectrometry. J Agr Food Chem. 2015;63(38):8592–600.
European Food Safety Authority. Scientific opinion on the risks for animal and public health related to the presence of T-2 and HT-2 toxin in food and feed. The EFSA J. 2011;9(12):2481. 1–187
Parent-Massin D. Haematotoxicity of trichothecenes. Toxicol Lett. 2004;153:75–81.
Liu Z, Gaoa J, Yuc J. Aflatoxins in stored maize and rice grains in Liaoning Province, China. J Stored Prod Res. 2006;42:468–79.
European Food Safety Authority. Opinion of the scientific panel on contaminants in the food chain on a request from the Commission related to the potential increase of consumer health risk by a possible increase of the existing maximum levels for aflatoxins in almonds, hazelnuts and pistachios and derived products. The EFSA J. 2007;446:1–127.
International Agency for Research on Cancer. IARC Monographs on the evaluation of carcinogenic risks to humans. Some naturally occurring substances: food items and constituents, heterocyclic aromatic amines and mycotoxins. Lyon, France; 1993. pp. 397–488.
International Agency for Research on Cancer. IARC Monographs on the evaluation of carcinogenic risks to humans. Some traditional herbal medicines, some mycotoxins, naphthalene and styrene. Lyon, France; 2002b. pp. 1–556.
Henry SH, Bosch FX, Bowers JC, Portier CJ, Petersen BJ, Barraj L. Aflatoxins. In: Safety Evaluation of Certain Food Additives and Contaminants, prepared by the Forty-ninth Meeting of the Joint FAO/WHO Expert Committee. FAO/WHO Food Additives Series 1999;40:361–468.
Commission Regulation (EU) No. 165/2010 of 26 February 2010 amending Regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuff as regards aflatoxins, Off J Eur Union, L 50, 8–12.
Commission Regulation (EC) No 1126/2007 of 28 September 2007 amending Regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuff as regards Fusarium toxins in maize and maize products, Off J Eur Union. L 255, 14–17.
Commission Recommendation (EU) No 165/2013 of 27 March 2013 on the presence of T-2 and HT-2 toxin in cereals and cereal products. Off J Eur Union, L 91, 12–15.
Imperato R, Campone C, Piccinelli AL, Veneziano A, Rastrelli L. Survey of aflatoxins and ochratoxin a contamination in food products imported in Italy. Food Control. 2011;22:1905–10.
Ruadrew S, Craft J, Aidoo K. Occurrence of toxigenic Aspergillus spp. and aflatoxins in selected food commodities of Asian origin sourced in the west of Scotland. Food Chem Toxicol. 2013;55:653–8.
Vaclavikova M, MacMahon S, Zhang K, Begley TH. Application of single immunoaffinity clean-up for simultaneous determination of regulated mycotoxins in cereals and nuts. Talanta. 2013;117:345–51.
Zhang Z, Hu X, Zhang Q, Li P. Determination for multiple mycotoxins in agricultural products using HPLC-MS/MS via a multiple antibody immunoaffinity column. J Chrom B. 2016;1021:145–52.
Lattanzio VMT, Ciasca B, Powers S, Visconti A. Improved method for the simultaneous determination of aflatoxins, ochratoxin A and fusarium toxins in cereals and derived product by liquid chromatography—tandem mass spectrometry after multi-toxin immunoaffinity clean up. J Chrom A. 2014;1354:139–43.
Berthiller F, Sulyok M, Krska R, Schuhmacher R. Chromatographic methods for the simultaneous determination of mycotoxins and their conjugates in cereals. Int J Food Microbiol. 2007;119:33–7.
Soleimany F, Jinap S, Abas F. Determination of mycotoxins in cereals by liquid chromatography tandem mass spectrometry. Food Chem. 2012;130:1055–60.
Oueslati S, Romero-González R, Lasram S, Garrido Frenich A, Martínez Vidal JL. 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. 2012;50:2376–81.
Alkadri D, Rubert J, Prodi A, Pisi A, Mañes J, Soler C. Natural co-occurrence of mycotoxins in wheat grains from Italy and Syria. Food Chem. 2014;157:111–8.
Commission Regulation (EU) No 519/2014 of 16 May 2014 amending Regulation (EC) No 401/2006 as regards methods of sampling of large lots, spices and food supplements, performance criteria for T-2, HT-2 toxin and citrinin and screening methods of analysis. Off J Eur Union, L 147, 29–43.
Bueno D, Istamboulie G, Muñoz R, Marty JL. Determination of mycotoxins in food: a review of bioanalytical to analytical methods. Appl Spectrosc Rev. 2015;50(9):728–74.
Köppen R, Koch M, Siegel D, Merkel S, Maul R, Nehls I. Determination of mycotoxins in foods: current state of analytical methods and limitations. Appl Microbiol Biotechnol. 2010;86(6):1595–612.
Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce. JAOAC Int. 2003;86(2):412–31.
Rubert J, Dzuman Z, Vaclavikova M, Zacharisova M, Soler C, Hajslova J. Analysis of mycotoxins in barley using ultra high liquid chromatography high resolution mass spectrometry: comparison of efficiency and efficacy of different extraction procedures. Talanta. 2012;99:712–9.
Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004 on official controls performed to ensure the verification of compliance with feed and food law, animal health and animal welfare rules. Off J Eur Communities, L191, 1–64.
Commission Decision of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of result. Off J Eur Union, L221, 8–36.
Antignac JP, De Wasch K, Monteau F, De Brabander H, Andre F, Le Bizec B. The ion suppression phenomenon in liquid chromatography–mass spectrometry and its consequences in the field of residue analysis. Anal Chim Acta. 2005;529:129–36.
EURACHEM/CITAC Guide. Quantifying uncertainty in analytical measurement, laboratory of government chemist. 3rd ed. 2012. pp. 1–133.
Vidal A, Marin S, Ramos AJ, Cano-Sancho G, Sanchis V. Determination of aflatoxins, deoxynivalenol, ochratoxin a and zearalenone in wheat and oat based bran supplements sold in the Spanish market. Food Chem Toxicol. 2013;53:133–8.
Liu Y, Lu Y, Wang L, Chang F, Yang L. Survey of 11 mycotoxins in wheat flour in Hebei province, China. Food Addit Contam B. 2015;8:250–4.
European Food Safety Authority. Aflatoxins (sum of B1, B2, G1, G2) in cereals and cereal-derived food products. Supporting publications. 2013;EN:406, pp. 1–11.
Trung TS, Tabuc C, Bailly S, Querin A, Guerre P, Bailly JD. Fungal mycoflora and contamination of maize from Vietnam with aflatoxin B1 and fumonisin B1. World Mycotoxin J. 2008;1(1):87–94.
Warth B, Parich A, Atehnkeng J, Bandyopadhyay R, Schuhmacher R, Sulyok M, et al. Quantitation of mycotoxins in food and feed from Burkina Faso and Mozambique using a modern LC-MS/MS multitoxin method. J Agr Food Chem. 2012;60:9352–63.
Giray B, Girgin G, Engin AB, Aydin S, Sahin G. Aflatoxin levels in wheat samples consumed in some regions of Turkey. Food Control. 2007;18:23–9.
Perenzin M, Cattaneo M, Rizzi E, Pedrotti A, Tonesi R. Frumento tenero biologico: Risultati agronomici e qualitativi. L’Informatore agrario. 2001;33:31-3.
Zinedine A, Juan C, Soriano JM, Moltó JC, Idrissi L, Mañes J. Limited survey for the occurrence of aflatoxins in cereals and poultry feeds from Rabat, Morocco. Int J Food Microbiol. 2007;115:124–7.
Zinedine A, Brera C, Elakhdari S, Catano C, Debegnach F, Angelini S, et al. Natural occurrence of mycotoxins in cereals and spices commercialized in Morocco. Food Control. 2006;17:868–74.
Schothorst RC, van Egmond HP. Report from SCOOP task 3.2.10 collection of occurrence data of Fusarium toxins in food and assessment of dietary intake by the population of EU member states, subtask: trichothecenes. Toxicol Lett. 2004;153:133–43.
Visconti A, Doko MB. Survey of fumonisin production by Fusarium isolated from cereals in Europe. J AOAC. 1994;77:546–50.
Bottalico A. Fusarium diseases of cereals: species complex and related mycotoxins profiles, in Europe. J Plant Pathol. 1998;80:85–103.
Shuaib FMB, Ehiri J, Abdullahi A, Williams JH, Jolly PE. Reproductive health effects of aflatoxins: a review of the literature. Reprod Toxicol. 2010;29:262–70.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declare that they have no conflict of interest.
Rights and permissions
About this article
Cite this article
Annunziata, L., Stramenga, A., Visciano, P. et al. Simultaneous determination of aflatoxins, T-2 and HT-2 toxins, and fumonisins in cereal-derived products by QuEChERS extraction coupled with LC-MS/MS. Anal Bioanal Chem 409, 5143–5155 (2017). https://doi.org/10.1007/s00216-017-0462-z
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00216-017-0462-z