Skip to main content
Springer Nature Link
Log in

Determination of Trichothecenes in Cereal Matrices Using Subcritical Water Extraction Followed by Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry

  • Published:
Food Analytical Methods Aims and scope Submit manuscript

Abstract

Subcritical water extraction followed by solid-phase extraction and ultra-high performance liquid chromatography coupled with tandem mass spectrometry detection is reported for the first time for the determination of 6 trichothecenes (deoxynivalenol, deoxynivalenol-3-glucoside, 3-acetyl-deoxynivalenol, 15-acetyl-deoxynivalenol, HT-2 toxin, and T-2 toxin) from different cereals. Water with 1% formic acid was used as the extraction solvent followed by a solid-phase extraction clean-up, achieving good performance with acceptable extraction recoveries, method detection limits between 0.05 μg kg−1 and 4.0 μg kg−1, and method quantification limits between 0.4 μg kg−1 and 20 μg kg−1. The use of water as the extraction solvent allowed a selective extraction affording low matrix effect levels and the detection and quantification of natural target trichothecenes at very low concentration levels. This extraction method was applied to different cereals, a pseudocereal and an oilseed sample, of which maize, millet, and oat were contaminated by at least one trichothecene.

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

Access this article

Log in via an institution

Subscribe and save

Springer+
from $39.99 /Month
  • Starting from 10 chapters or articles per month
  • Access and download chapters and articles from more than 300k books and 2,500 journals
  • Cancel anytime
View plans

Buy Now

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1

Similar content being viewed by others

Explore related subjects

Discover the latest articles, books and news in related subjects, suggested using machine learning.

References

  • Ačanski MM, Vujić DN, Psodorov DB (2015) Practical method for the confirmation of authentic flours of different types of cereals and pseudocereals. Food Chem 172:314–317

    Article  Google Scholar 

  • Arendt E, Dal Bello F (2008) Gluten-free cereal products and beverages. Food Sci Technol 4-8:81–190

    Google Scholar 

  • Armenta S, Garrigues S, de la Guardia M (2015) The role of green extraction techniques in Green Analytical Chemistry. Trends Anal Chem 71:2–8

    Article  CAS  Google Scholar 

  • Berthiller F, Crews C, Dall’Asta C et al (2013) Masked mycotoxins: a review. Mol Nutr Food Res 57:165–186

    Article  CAS  Google Scholar 

  • Campone L, Piccinelli AL, Celano R et al (2015) A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry. Anal Bioanal Chem 407:2899–2911

    Article  CAS  Google Scholar 

  • Commission Recommendation EC (2013) No 2013/165/EU of 27 March 2013 on the presence of T-2 and HT-2 toxin in cereals and cereal products. Off J Eur Union L91:12–15

    Google Scholar 

  • Commission Regulation EC (2007) No 1126/2007 of 28 September 2007 amending regulation (EC) No 1881/2006 setting maximum levels for certain contaminants in foodstuffs as regards Fusarium toxins in maize and maize products. Off J Eur Union L255:14–17

    Google Scholar 

  • Desmarchelier A, Oberson J-M, Tella P et al (2010) Development and comparison of two multiresidue methods for the analysis of 17 mycotoxins in cereals by liquid chromatography electrospray ionization tandem mass spectrometry. J Agric Food Chem 58:7510–7519

    Article  CAS  Google Scholar 

  • European Food Safety Authority, EFSA-Q-2013-00721 (2013a) Request for a scientific opinion on the risks for animals and public health related to the presence of deoxynivalenol, metabolites of deoxynivalenol and masked deoxynivalenol in food and feed. Available at www.efsa.europa.eu. Accessed 12 Mar 2017

  • European Food Safety Authority, EFSA (2013b) Deoxynivalenol in food and feed: occurrence and exposure. EFSA J 11:3379–3434

    Google Scholar 

  • Gottschalk C, Barthel J, Engelhardt G et al (2007) Occurrence of type a trichothecenes in conventionally and organically produced oats and oat products. Mol Nutr Food Res 51:1547–1553

    Article  CAS  Google Scholar 

  • Herrero M, Castro-Puyana M, Mendiola JA, Ibañez E (2013) Compressed fluids for the extraction of bioactive compounds. Trends Anal Chem 43:67–83

    Article  CAS  Google Scholar 

  • Jestoi M, Somma MC, Kouva M et al (2004) Levels of mycotoxins and sample cytotoxicity of selected organic and conventional grain-based products purchased from Finnish and Italian markets. Mol Nutr Food Res 48:299–307

    Article  CAS  Google Scholar 

  • JiaoJiao X, Jian Z, BaiFen H et al (2016) Simultaneous and rapid determination of deoxynivalenol and its acetylate derivatives in wheat flour and rice by ultra high performance liquid chromatography with photo diode array detection. J Sep Sci 39:2028–2035

    Article  Google Scholar 

  • Joint FAO/WHO Expert Committe on Food Additives, JECFA (2011) Evaluation of certain contaminants in food. World Heal Organ Tech Rep Ser 959:1–105

    Google Scholar 

  • Juan C, Ritieni A, Mañes J (2013) Occurrence of Fusarium mycotoxins in Italian cereal and cereal products from organic farming. Food Chem 141:1747–1755

    Article  CAS  Google Scholar 

  • Kokkonen MK, Jestoi MN (2009) A multi-compound LC-MS/MS method for the screening of mycotoxins in grains. Food Anal Methods 2:128–140

    Article  Google Scholar 

  • Kostelanska M, Dzuman Z, Malachova A et al (2011) Effects of milling and baking technologies on levels of deoxynivalenol and its masked form deoxynivalenol-3-glucoside. J Agric Food Chem 59:9303–9312

    Article  CAS  Google Scholar 

  • Krska R, Welzig E, Boudra H (2007) Analysis of Fusarium toxins in feed. Anim Feed Sci Technol 137:241–264

    Article  CAS  Google Scholar 

  • Krysińska-Traczyk E, Perkowski J, Dutkiewicz J (2007) Levels of fungi and mycotoxins in the samples of grain and grain dust collected from five various cereal crops in eastern Poland. Ann Agric Environ Med 14:159–167

    Google Scholar 

  • Maresca M (2013) From the gut to the brain: journey and pathophysiological effects of the food-associated trichothecene mycotoxin deoxynivalenol. Toxins (Basel) 5:784–820

    Article  CAS  Google Scholar 

  • Miró-Abella E, Herrero P, Canela N et al (2017) Determination of mycotoxins in plant-based beverages using QuEChERS and liquid chromatography-tandem mass spectrometry. Food Chem 229:366–372

    Article  Google Scholar 

  • Nagl V, Woechtl B, Schwartz-Zimmermann HE et al (2014) Metabolism of the masked mycotoxin deoxynivalenol-3-glucoside in pigs. Toxicol Lett 229:190–197

    Article  CAS  Google Scholar 

  • Pallaroni L, Von Holst C (2003) Comparison of alternative and conventional extraction techniques for the determination of zearalenone in corn. Anal Bioanal Chem 376:908–912

    Article  CAS  Google Scholar 

  • Pallaroni L, Von Holst C, Eskilsson CS, Björklund E (2002) Microwave-assisted extraction of zearalenone from wheat and corn. Anal Bioanal Chem 374:161–166

    Article  CAS  Google Scholar 

  • Payros D, Alassane-Kpembi I, Pierron A et al (2016) Toxicology of deoxynivalenol and its acetylated and modified forms. Arch Toxicol 90:2931–2957

    Article  CAS  Google Scholar 

  • Pereira VL, Fernandes JO, Cunha SC (2014) Mycotoxins in cereals and related foodstuffs: a review on occurrence and recent methods of analysis. Trends Food Sci Technol 36:96–136

    Article  CAS  Google Scholar 

  • Pestka JJ (2008) Mechanisms of deoxynivalenol-induced gene expression and apoptosis. Food Addit Contam Part A Chem Anal Control Expo Risk Assess 25:1128–1140

    Article  CAS  Google Scholar 

  • Plaza M, Turner C (2015) Pressurized hot water extraction of bioactives. Trends Anal Chem 71:39–54

    Article  CAS  Google Scholar 

  • Rubert J, Soriano JM, Mañes J, Soler C (2013) Occurrence of fumonisins in organic and conventional cereal-based products commercialized in France, Germany and Spain. Food Chem Toxicol 56:387–391

    Article  CAS  Google Scholar 

  • Rubert J, León N, Sáez C et al (2014) Evaluation of mycotoxins and their metabolites in human breast milk using liquid chromatography coupled to high resolution mass spectrometry. Anal Chim Acta 820:39–46

    Article  CAS  Google Scholar 

  • Sánchez Maldonado AF, Mudge E, Gänzle MG, Schieber A (2014) Extraction and fractionation of phenolic acids and glycoalkaloids from potato peels using acidified water/ethanol-based solvents. Food Res Int 65:27–34

    Article  Google Scholar 

  • SANTE (2015) European Commission Document No SANTE/11945/2015. Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed

  • Schollenberger M, Müller HM, Rüfle M et al (2005) Survey of Fusarium toxins in foodstuffs of plant origin marketed in Germany. Int J Food Microbiol 97:317–326

    Article  CAS  Google Scholar 

  • Teo CC, Tan SN, Yong JWH et al (2010) Pressurized hot water extraction (PHWE). J Chromatogr A 1217:2484–2494

    Article  CAS  Google Scholar 

  • Veprikova Z, Zachariasova M, Dzuman Z et al (2015) Mycotoxins in plant-based dietary supplements: hidden health risk for consumers. J Agric Food Chem 63:6633–6643

    Article  CAS  Google Scholar 

  • Zachariasova M, Lacina O, Malachova A et al (2010) Novel approaches in analysis of fusarium mycotoxins in cereals employing ultra performance liquid chromatography coupled with high resolution mass spectrometry. Anal Chim Acta 662:51–61

    Article  CAS  Google Scholar 

  • Zhou Q, Li F, Chen L, Jiang D (2016) Quantitative analysis of 10 mycotoxins in wheat flour by ultrahigh performance liquid chromatography-tandem mass spectrometry with a modified QuEChERS strategy. J Food Sci 81:T2886–T2890

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Department of Analytical Chemistry and Organic Chemistry, Universitat Rovira i Virgili, Sescelades Campus, Marcel·lí Domingo, s/n, 43007, Tarragona, Spain

    Eugènia Miró-Abella, Núria Fontanals & Francesc Borrull

  2. Group of Research on Omic Methodologies (GROM), Centre for Omic Sciences (COS), Universitat Rovira i Virgili, Av. Universitat 1, 43204, Reus, Spain

    Eugènia Miró-Abella, Pol Herrero, Núria Canela & Rosa Ras

  3. Unitat de biotecnologia–EURECAT, Av. Universitat 1, 43204, Reus, Spain

    Lluís Arola

Authors
  1. Eugènia Miró-Abella
    View author publications

    Search author on:PubMed Google Scholar

  2. Pol Herrero
    View author publications

    Search author on:PubMed Google Scholar

  3. Núria Canela
    View author publications

    Search author on:PubMed Google Scholar

  4. Lluís Arola
    View author publications

    Search author on:PubMed Google Scholar

  5. Rosa Ras
    View author publications

    Search author on:PubMed Google Scholar

  6. Núria Fontanals
    View author publications

    Search author on:PubMed Google Scholar

  7. Francesc Borrull
    View author publications

    Search author on:PubMed Google Scholar

Corresponding author

Correspondence to Núria Fontanals.

Ethics declarations

Conflict of Interest

Eugènia Miró-Abella declares that she has no conflict of interest. Pol Herrero declares that he has no conflict of interest. Núria Canela declares that she has no conflict of interest. Lluís Arola declares that he has no conflict of interest. Rosa Ras declares that she has no conflict of interest. Núria Fontanals declares that she has no conflict of interest. Francesc Borrull declares that he has no conflict of interest.

Research Involving Human Participants and/or Animals

ᅟ

Ethical Approval

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

Informed Consent

Not applicable.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Miró-Abella, E., Herrero, P., Canela, N. et al. Determination of Trichothecenes in Cereal Matrices Using Subcritical Water Extraction Followed by Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry. Food Anal. Methods 11, 1113–1121 (2018). https://doi.org/10.1007/s12161-017-1089-6

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s12161-017-1089-6

Keywords