Analytical and Bioanalytical Chemistry

, Volume 381, Issue 8, pp 1592–1595 | Cite as

Determination of ochratoxin A in wine by liquid chromatography tandem mass spectrometry after combined anion-exchange/reversed-phase clean-up

Original Paper


Ochratoxin A (OTA) is a mycotoxin produced by Aspergillus ochraceus and Penicillium verrucosum. It has been found and analysed in several foods and feeds. Owing to its toxicity and occurrence in food and feed, the European Community has issued directives and some countries have their own regulations for OTA contents in food, feed and beverages. This work describes a method for the determination of OTA in mulled and red wine. It is based on combined anion exchange/reversed-phase clean-up and was analysed by liquid chromatography coupled with tandem mass spectrometry (multiple reaction monitoring). The method was validated with natural contaminated and spiked wine samples with OTA contents from 1.34 to 3.48 μg kg−1. Owing to its accuracy, good reproducibility and repeatability, this easy method is a good alternative to liquid chromatography–fluorescence detection methods.


Ochratoxin A Wine Tandem mass spectrometry Solid-phase extraction Anion exchange Liquid chromatography 


  1. 1.
    van der Merwe KJ, Steyn PS, Fourie L, Scott DB, Theron JJ (1965) Wilh Nat 205:1112–1113Google Scholar
  2. 2.
    Bedele AM, Carlton WW, Krogh P, Lillehoj EB (1985) J Natl Cancer 75:773–742Google Scholar
  3. 3.
    Imaida K, Hirose M, Ogiso T, Kurata Y, Ito N (1982) Cancer Lett 16:137–143Google Scholar
  4. 4.
    Bruinink A, Sidler C (1997) Toxicol Appl Pharmacol 146:173–179Google Scholar
  5. 5.
    Thuvander A, Funseth E, Breitholtz-Emanuelsson A, Hallén Palmiger I, Oskarsson A (1996b) Nat Toxins 141–147Google Scholar
  6. 6.
    IARC Monographs on the evaluation of carcinogenic risks to humans (1993) International Agency for Research on Cancer, Geneva 56:489–521Google Scholar
  7. 7.
    Leitner A, Zöllner P, Paolillo A, Stroka J, Papadopoulou-Bouraoui A, Jaborek S, Anklam E, Lindner W (2002) Anal Chim Acta 453:33–41Google Scholar
  8. 8.
    Nakajima M, Tsubouchi H, Miyabe M (1999) J AOAC Int 82(4):897–902Google Scholar
  9. 9.
    Solfrizzo M, Avantaggiato G, Viscont A (1998) J Chromatogr A 815:67–73Google Scholar
  10. 10.
    Bauer J, Gareis M (1987) J Vet Med B 34:613–627Google Scholar
  11. 11.
    Commision Regulation (EC) No 472/2002 of 12 March 2002 Amending Regulation (EC) No 466/2001 setting maximum levels for certain contaminants in foodstuffsGoogle Scholar
  12. 12.
    Verordnung zur Änderung der Mykotoxin-Höchstmengenverordnung und der Diätverordnung vom 04.02.2004Google Scholar
  13. 13.
    Visconti A, Pascale M, Centonze G (2000) J Chromatogr A 888:321–326Google Scholar
  14. 14.
    DIN EN14133: determination of ochratoxin A in wine and beer-HPLC method with immunoaffinity column clean-upGoogle Scholar
  15. 15.
    DIN EN14132: determination of ochratoxin A in barley and roasted coffee-HPLC method with immunoaffinity column clean-upGoogle Scholar
  16. 16.
    EN ISO 15141-1 Determination of ochratoxin A in cereals and cereal products-Part 1: high performance liquid chromatographic method with silica gel clean upGoogle Scholar
  17. 17.
    Lau BPY, Scott PM, Lewis DA, Kanhere SR (2000) J Mass Spectrom 35:23–32Google Scholar
  18. 18.
    Jornet D, Busto O, Guash J (2000) J Chromatogr A 882:29–35CrossRefGoogle Scholar
  19. 19.
    Saez JM, Medina A, Gimeno-Adelantado JV, Mateo R, Jimenez M (2004) J Chromatogr A 1029:125–133CrossRefGoogle Scholar
  20. 20.
    Uchiyama S, Saito Y, Uchiyama M (1985) J Food Hyg Soc Jpn 26:651Google Scholar
  21. 21.
    DIN 32645 Chemical analysis; Decision limit, detection limit and determination limit; Estimation in case of repeatability, terms, methods, evaluationGoogle Scholar

Copyright information

© Springer-Verlag 2005

Authors and Affiliations

  1. 1.Department of Analytical ChemistryFederal Institute for Materials Research and TestingBerlinGermany

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