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Analytical and Bioanalytical Chemistry

, Volume 399, Issue 3, pp 1279–1286 | Cite as

Dispersive liquid–liquid microextraction combined with high-performance liquid chromatography–tandem mass spectrometry for the identification and the accurate quantification by isotope dilution assay of Ochratoxin A in wine samples

  • Luca Campone
  • Anna Lisa Piccinelli
  • Luca Rastrelli
Original Paper

Abstract

A novel approach for the rapid analysis of ochratoxin A (OTA) in wine samples is presented. Mycotoxin was extracted and concentrated from matrix using dispersive liquid–liquid microextraction (DLLME). The final extract is analyzed by liquid chromatography coupled to positive electrospray ionization tandem mass spectrometry employing [2H5]-ochratoxin A as internal standard. Some important parameters, such as the nature and volume of extraction solvent and dispersive solvent, and salt effect were investigated and optimized to achieve the best extraction efficiency and higher enrichment factor. Under the optimum extraction condition, the method provided enrichment factor around 80 times and showed a high sensitivity with method detection and quantification limits of 0.005 and 0.015 ng mL−1, respectively. To test the accuracy of the analytical procedure, the optimized method was applied to the analysis of reference material T1755 (naturally contaminated white wine), with excellent results (accuracy of 103%) and showing a good precision with a CV (n = 6) of 5.8%. The proposed method, which is demonstrated to be quick, cheap, accurate and highly selective, was successfully applied to the analysis of Italian wines.

Figure

Analysis of ochratoxin A in wine by DLLME coupled to LC-MS/MS

Keywords

Ochratoxin A Wine Dispersive liquid–liquid microextraction HPLC-MS/MS Isotope dilution 

References

  1. 1.
    Pfohl-Leszkowicz A, Manderville R (2007) Mol Nutr Food Res 51:61–99CrossRefGoogle Scholar
  2. 2.
    O’Brien E, Dietrich D (2005) CRC Crit Rev Toxicol 35:33–60CrossRefGoogle Scholar
  3. 3.
    Evaluation of certain Mycotoxins: Ochratoxin A, WHO food additives series 47/FAO food and nutrition paper 74, 2001Google Scholar
  4. 4.
    Petkova-Botcharova T, Chernozemsky IN, Castegnaro M (1988) Food Addit Contam 5:299–301CrossRefGoogle Scholar
  5. 5.
    IARC Monographs on the evaluation of carcinogenic risks to humans, vol 56: 489, IARC, Geneva, Switzerland, 1993Google Scholar
  6. 6.
    EFSA 2006. European food safety authority. Opinion of the scientific panel on contaminants in the food chain of the EFSA on a request from the commission related to ochratoxin A in food. (2006)EFSA J 365: 1Google Scholar
  7. 7.
    Commission Regulation (EC) 1881/2006 (2006) Off J Eur Union L 364:5–24Google Scholar
  8. 8.
    Mateo R, Medina Á, Mateo EM, Mateo F, Jiménez M (2007) Int J Food Microbiol 119:79–83CrossRefGoogle Scholar
  9. 9.
    Visconti A, Perrone G, Cozzi G, Solfrizzo M (2008) Food Addit Contam 25:193–202CrossRefGoogle Scholar
  10. 10.
    Monaci L, Palmisano F (2004) Anal Bioanal Chem 378:96–103CrossRefGoogle Scholar
  11. 11.
    Barna Vetro I, Solti L, Teren L, Gyongyosi A, Szabo E, Wolfling A (1996) J Agric Food Chem 44:4071–4074CrossRefGoogle Scholar
  12. 12.
    Flajs D, Domijan AM, Ivic D, Cvjetkovic B, Peraica M (2009) Food Control 20:590–592CrossRefGoogle Scholar
  13. 13.
    Valenta H (1998) J Chromatogr A 815:75–92CrossRefGoogle Scholar
  14. 14.
    Visconti A, Pascale M, Centonze G (2001) J AOAC Int 84:1818–1827Google Scholar
  15. 15.
    Flamini R, Panighel A (2006) Mass Spectrom Rev 25:741–774CrossRefGoogle Scholar
  16. 16.
    Leitner A, Zöllner P, Paolillo A, Stroka J, Papadopoulou-Bouraoui A, Jaborek S, Anklam E, Lindner W (2002) Anal Chim Acta 453:33–41CrossRefGoogle Scholar
  17. 17.
    Bacaloni A, Cavaliere C, Faberi A, Pastorini E, Samperi R, Laganà A (2005) J Agric Food Chem 53:5518–5525CrossRefGoogle Scholar
  18. 18.
    Rychlik M, Asam S (2008) Anal Bioanal Chem 390:617–628CrossRefGoogle Scholar
  19. 19.
    Stokvis E, Rosing H, Beijnen JH (2005) Rapid Commun Mass Spectrom 19:401–407CrossRefGoogle Scholar
  20. 20.
    Rezaee M, Assadi Y, Hosseini MRM, Aghaee E, Ahmadi F, Berijani S (2006) J Chromatogr A 1116:1–9CrossRefGoogle Scholar
  21. 21.
    Nagaraju D, Huang S-D (2007) J Chromatogr A 1161:89–97CrossRefGoogle Scholar
  22. 22.
    García-López M, Rodríguez I, Cela R (2007) J Chromatogr A 1166:9–15CrossRefGoogle Scholar
  23. 23.
    Rezaee M, Yamini Y, Shariati S, Esrafili A, Shamsipur M (2009) J Chromatogr A 1216:1511–1514CrossRefGoogle Scholar
  24. 24.
    Fattahi N, Samadi S, Assadi Y, Hosseini MRM (2007) J Chromatogr A 1169:63–69CrossRefGoogle Scholar
  25. 25.
    Montes R, Rodríguez I, Ramil M, Rubí E, Cela R (2009) J Chromatogr A 1216:5459–5466CrossRefGoogle Scholar
  26. 26.
    Zhao E, Zhao W, Han L, Jiang S, Zhou Z (2007) J Chromatogr A 1175:137–140CrossRefGoogle Scholar
  27. 27.
    Commission Decision 2002/657/EC (2002) Off J Eur Communities L 221:8–36Google Scholar
  28. 28.
    Commission Regulation (EC) 401/2006 (2006) Off J Eur Union L 70:12–34Google Scholar

Copyright information

© Springer-Verlag 2010

Authors and Affiliations

  • Luca Campone
    • 1
  • Anna Lisa Piccinelli
    • 1
  • Luca Rastrelli
    • 1
  1. 1.Dipartimento di Scienze Farmaceutiche (DIFARMA)Università degli Studi di SalernoFiscianoItaly

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