Skip to main content

Determination of Deoxynivalenol and Its Derivative in Corn Flour and Wheat Flour Using Automated On-line Solid-Phase Extraction Combined with LC–MS/MS

Abstract

An automated on-line solid-phase extraction (SPE) combined with LC–MS/MS method was developed for determination of deoxynivalenol (DON), 3-acetyl-DON and 15-acetyl-DON in corn flour and wheat flour samples. The extraction solvent of the samples was injected into the automated on-line SPE system to remove matrix interference. After washing step, the targets were eluted from the SPE cartridge into liquid chromatography (LC) column. Several SPE parameters including injection volume, elution volume and eluting flow rate were assessed and optimized. Method validation was evaluated and good linearity was obtained (R2 > 99%) with the limit of detection of 0.1–0.2 μg/kg. Recoveries were evaluated in spiked corn flour and wheat flour samples at three concentrations and the values ranged from 86.5% to 99.7%. The benefit of the present method with automated on-line SPE system is the ability to inject directly pure extracts into LC–MS/MS, offering faster analyses and improving analysis efficiency.

This is a preview of subscription content, access via your institution.

Fig. 1
Fig. 2
Fig. 3

References

  1. Alizadeh A, Braber S, Akbari P, Kraneveld A, Garssen J, Fink-Gremmels J (2016) Deoxynivalenol and its modified forms: are there major differences? Toxins 8(11):334

    Article  Google Scholar 

  2. Bourgogne E, Grivet C, Varesio E, Hopfgartner G (2015) Generic on-line solid phaseextraction sample preparation strategies for the analysis of drugs in biological matrices by LC-MS/MS. J Pharmaceut Biomed 102:290–298

    CAS  Article  Google Scholar 

  3. Broekaert N, Devreese M, De Mil T, Fraeyman S, De Baere S, De Saeger S, De Backer P, Croubels S (2014) Development and validation of an LC-MS/MS method for the toxicokinetic study of deoxynivalenol and its acetylated derivatives in chicken and pig plasma. J Chromatogr B 971:43–51

    CAS  Article  Google Scholar 

  4. Campone L, Piccinelli AL, Celano R, Pagano I, Russo M, Rastrelli L (2018) Rapid and automated on-line solid phase extraction HPLC-MS/MS with peak focusing for the determination of ochratoxin A in wine samples. Food Chem 244:128–135

    CAS  Article  Google Scholar 

  5. European Commission (2006) Commission Regulation (EC) No. 1881/2006 of 19 December 2006 setting maximum levels for certain contaminants in foodstuffs. In: Commission, E. (ed.) pp. 2–8. Official Journal of the European Union L.

  6. Fang GZ, He JX, Wang S (2006) Multiwalled carbon nanotubes as sorbent for on-line coupling of solid-phase extraction to high-performance liquid chromatography for simultaneous determination of 10 sulfonamides in eggs and pork. J Chromatogr A 1127(1–2):12–17

    CAS  Article  Google Scholar 

  7. Ferrer-Aguirre A, Romero-González R, Vidal JM, Frenich AG (2016) Simple and quick determination of analgesics and other contaminants of emerging concern in environmental waters by on-line solid phase extraction coupled to liquid chromatography-tandem mass spectrometry. J Chromatogr A 1446:27–33

    CAS  Article  Google Scholar 

  8. Gerez JR, Pinton P, Callu P, Grosjean F, Oswald IP, Bracarense APF (2015) Deoxynivalenol alone or in combination with nivalenol and zearalenone induce systemic histological changes in pigs. Exp Toxicol Pathol 67(2):89–98

    CAS  Article  Google Scholar 

  9. Gonçalves C, Stroka J (2016) Cross-reactivity features of deoxynivalenol (DON)-targeted immunoaffinity columns aiming to achieve simultaneous analysis of DON and major conjugates in cereal samples. Food Addit Contam A 33(6):1053–1062

    Article  Google Scholar 

  10. Ibáñez-Vea M, Lizarraga E, González-Peñas E (2011) Simultaneous determination of type-A and type-B trichothecenes in barley samples by GC-MS. Food Control 22(8):1428–1434

    Article  Google Scholar 

  11. ICH, Q2 (R1) Harmonised Tripartite Guideline (2005). Validation of analytical procedure: text and methodology. In: International Conference on Harmonization, Geneva.

  12. Liu Y, Lu Y, Wang L, Chang F, Yang L (2016) Occurrence of deoxynivalenol in wheat, Hebei Province, China. Food Chem 197:1271–1274

    CAS  Article  Google Scholar 

  13. Li X, Xiao H, Liang X, Shi D, Liu J (2004) LC-MS/MS determination of naringin, hesperidin and neohesperidin in rat serum after orally administrating the decoction of Bulpleurum falcatum L. and Fractus aurantii. J Pharmaceut Biomed 34(1):159–166

    CAS  Article  Google Scholar 

  14. Mateo JJ, Llorens A, Mateo R, Jiménez M (2001) Critical study of and improvements in chromatographic methods for the analysis of type b trichothecenes. J Chromatogr A 918(1):99–112

    CAS  Article  Google Scholar 

  15. Mi J, Li S, Xu H, Liang W, Sun T (2014) Rapid analysis of three β-agonist residues in food of animal origin by automated on-line solid-phase extraction coupled to liquid chromatography and tandem mass spectrometry. J Sep Sci 37(17):2431–2438

    CAS  Article  Google Scholar 

  16. Mishra S, Srivastava S, Dewangan J, Divakar A, Rath SK (2020) Global occurrence of deoxynivalenol in food commodities and exposure risk assessment in humans in the last decade: a survey. Crit Rev Food Sci 8:1346–1374

    Article  Google Scholar 

  17. Olcer Z, Esen E, Muhammad T, Ersoy A, Budak S, Uludag Y (2014) Fast and sensitive detection of mycotoxins in wheat using microfluidics based real-time electrochemical profiling. Biosens Bioelectron 62:163–169

    CAS  Article  Google Scholar 

  18. Rahmani M, Ghasemi E, Sasani M (2017) Application of response surface methodology for air assisted-dispersive liquid-liquid microextraction of deoxynivalenol in rice samples prior to HPLC-DAD analysis and comparison with solid phase extraction cleanup. Talanta 165:27–32

    CAS  Article  Google Scholar 

  19. Ran R, Wang C, Han Z, Wu A, Zhang D, Shi J (2013) Determination of deoxynivalenol (DON) and its derivatives: current status of analytical methods. Food Control 34(1):138–148

    CAS  Article  Google Scholar 

  20. Rodríguez-Carrasco Y, Moltó JC, Mañes J, Berrada H (2017) Development of microextraction techniques in combination with GC-MS/MS for the determination of mycotoxins and metabolites in human urine. J Sep Sci 40(7):1572–1582

    Article  Google Scholar 

  21. Rossi E, Errea MI, de Cortalezzi MMF, Stripeikis J (2017) Selective determination of Cr (VI) by on-line solid phase extraction FI-SPE-FAAS using an ion exchanger resin as sorbent: an improvement treatment of the analytical signal. Microchem J 130:88–92

    CAS  Article  Google Scholar 

  22. Salazar-Beltrán D, Hinojosa-Reyes L, Ruiz-Ruiz E, Hernández-Ramírez A, Guzmán-Mar JL (2017) Determination of phthalates in bottled water by automated on-line solid phase extraction coupled to liquid chromatography with uv detection. Talanta 168:291–297

    Article  Google Scholar 

  23. Sanchís J, Kantiani L, Llorca M, Rubio F, Ginebreda A, Fraile J, Garrido T, Farré M (2012) Determination of glyphosate in groundwater samples using an ultrasensitive immunoassay and confirmation by on-line solid-phase extraction followed by liquid chromatography coupled to tandem mass spectrometry. Anal Bioanal Chem 402(7):2335–2345

    Article  Google Scholar 

  24. Tang K, Liu H, Li XZ, Hassan YI, Shao S, Zhou T (2018) An efficient gas chromatography-mass spectrometry approach for the simultaneous analysis of deoxynivalenol and its bacterial metabolites 3-keto-DON and 3-epi-DON. J Food Protect 81(2):233–239

    CAS  Article  Google Scholar 

  25. Tralamazza SM, Bemvenuti RH, Zorzete P, de Souza GF, Corrêa B (2016) Fungal diversity and natural occurrence of deoxynivalenol and zearalenone in freshly harvested wheat grains from Brazil. Food Chem 196:445–450

    CAS  Article  Google Scholar 

  26. USP 29/NF 24 the United States Pharmacopoeia (2006) 29 the Rev. and the National Formulary (pp. 1964–1966). United States Pharmacopoeial Convention Inc., Rockville

  27. Wu Q, Kuča K, Humpf HU, Klímová B, Cramer B (2017) Fate of deoxynivalenol and deoxynivalenol-3-glucoside during cereal-based thermal food processing: a review study. Mycotoxin Res 33(1):79–91

    CAS  Article  Google Scholar 

  28. Wu W, Zhang H (2014) Role of tumor necrosis factor-α and interleukin-1β in anorexia induction following oral exposure to the trichothecene deoxynivalenol (vomitoxin) in the mouse. J Toxicol Sci 39(6):875–886

    CAS  Article  Google Scholar 

  29. Ye X, Tao LJ, Needham LL, Calafat AM (2008) Automated on-line column-switching HPLC-MS/MS method for measuring environmental phenols and parabens in serum. Talanta 76(4):865–871

    CAS  Article  Google Scholar 

  30. Yoshinari T, Ohnishi T, Kadota T, Sugita-Konishi Y (2012) Development of a purification method for simultaneous determination of deoxynivalenol and its acetylated and glycosylated derivatives in corn grits and corn flour by liquid chromatography-tandem mass spectrometry. J Food Protect 75(7):1355–1358

    CAS  Article  Google Scholar 

  31. Yuan J, Sun C, Guo X, Yang T, Wang H, Fu S, Li C, Yang H (2017) A rapid Raman detection of deoxynivalenol in agricultural products. Food Chem 221:797–802

    CAS  Article  Google Scholar 

  32. Zhang H, Sun J, Zhang Y, Lu M, Sun L, Li W, Hu X, Wang B (2016) Retention of deoxynivalenol and its derivatives during storage of wheat grain and flour. Food Control 65:177–181

    CAS  Article  Google Scholar 

  33. Zhou X, Kramer JP, Calafat AM, Ye X (2014) Automated on-line column-switching high performance liquid chromatography isotope dilution tandem mass spectrometry method for the quantification of bisphenol A, bisphenol F, bisphenol S, and 11 other phenols in urine. J Chromatogr B 944:152–156

    CAS  Article  Google Scholar 

Download references

Acknowledgements

This work was supported by the National Key R&D Program of China (No. 2017YFF0211300) and the Scientific Research Foundation for the Introduced Talent of Hebei Agricultural University (No. YJ201911).

Author information

Affiliations

Authors

Corresponding author

Correspondence to Yiwei Tang.

Additional information

Publisher's Note

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

Electronic supplementary material

Below is the link to the electronic supplementary material.

Supplementary file1 (DOCX 493 kb)

Rights and permissions

Reprints and Permissions

About this article

Verify currency and authenticity via CrossMark

Cite this article

Cao, M., Li, Q., Zhang, Y. et al. Determination of Deoxynivalenol and Its Derivative in Corn Flour and Wheat Flour Using Automated On-line Solid-Phase Extraction Combined with LC–MS/MS. Bull Environ Contam Toxicol 107, 248–254 (2021). https://doi.org/10.1007/s00128-020-02920-y

Download citation

Keywords

  • Deoxynivalenol
  • Automated on-line solid-phase extraction
  • LC–MS/MS
  • Corn flour
  • Wheat flour