Advertisement

Analytical and Bioanalytical Chemistry

, Volume 405, Issue 26, pp 8645–8652 | Cite as

Rapid analysis of aflatoxin M1 in milk using dispersive liquid–liquid microextraction coupled with ultrahigh pressure liquid chromatography tandem mass spectrometry

  • Luca Campone
  • Anna Lisa PiccinelliEmail author
  • Rita Celano
  • Mariateresa Russo
  • Luca Rastrelli
Research Paper

Abstract

A simple, rapid, and sensitive method based on simultaneous protein precipitation and extraction of aflatoxin M1 (AFM1) followed by dispersive liquid–liquid microextraction (DLLME) and ultrahigh pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) analysis was developed for the determination of AFM1 in milk samples. In order to precipitate the proteins and extract AFM1 from milk, a sample pretreatment using acetonitrile and NaCl as the extraction/denaturant solvent and salting-out agent, respectively, was optimised. Subsequently, the acetonitrile (upper) phase, containing AFM1, was used as the disperser solvent in DLLME, and extractant (chloroform) and water were added in turn to the extract to perform the DLLME process. The main parameters affecting the extraction efficiency of the whole analytical procedure, such as acetonitrile volume, amount of salt, type and volume of extractant and water volume, were carefully optimised by experimental design. Under optimum conditions, the developed method provides an enrichment factor of 33 and detection and quantification limits (0.6 and 2.0 ng kg−1, respectively) below the maximum levels imposed by current regulations for AFM1 in milk and infant milk formulae. Recoveries (61.3–75.3 %) and repeatability (RSD < 10, n = 3), tested in different types of milk at four AFM1 levels, met the performance criteria required by EC Regulation No. 401/2006. Moreover, the matrix effect on the signal intensity of the analyte was negligible. The proposed method provides a rapid extraction and an accurate determination of AFM1 in milk and formula milk using a simple and inexpensive sample preparation procedure.

Figure

Rapid analysis of aflatoxin M1 in milk using DLLME

Keywords

Milk Aflatoxin M1 Protein precipitation Dispersive liquid–liquid microextraction UHPLC-MS/MS 

Notes

Acknowledgements

The Project was funded by the Italian Ministry of the University and Research (MIUR) with a FIRB “Futuro in Ricerca” Project n. RBFR10GSJK “Tecniche Analitiche Avanzate per l’Analisi dei Contaminanti negli Alimenti”.

References

  1. 1.
    FAO/WHO (1997) WHO Tech Rep Ser 868:1–69Google Scholar
  2. 2.
    IARC (1993) IARC Monogr Eval Carcinog Risks Hum 56:245–395Google Scholar
  3. 3.
    IARC (2002) IARC Monogr Eval Carcinog Risks Hum 82:171–30Google Scholar
  4. 4.
    Van Egmond HP (1989) In: van Egmond HP (ed) Mycotoxins in dairy products, aflatoxin M1: occurrence, toxicity, regulation. Amsterdam, ElsevierGoogle Scholar
  5. 5.
    Prandini A, Tansini G, Sigolo S, Filippi L, Laporta M, Piva G (2009) Food Chem Toxic 47:984–991CrossRefGoogle Scholar
  6. 6.
    Veldman A, Meijst JAC, Borggreve GJ (1992) Heeres-van der Tol JJ. Anim Prod 55:163–168CrossRefGoogle Scholar
  7. 7.
    European Food Safety Authority. Opinion of the scientific panel on contaminants in the food chain on a request from the Commission related to aflatoxin B1 as undesirable substance in animal feed. (2004) EFSA J 39:1−27Google Scholar
  8. 8.
    Commission Regulation (EC) 1881/2006 (2006)) Off J Eur Union L 364:5–24Google Scholar
  9. 9.
    Muscarella M, Magro S, Palermo C, Centonze D (2007) Anal Chim Acta 594:257–264CrossRefGoogle Scholar
  10. 10.
    Commission Decision 2002/657/EC (2002) Off J Eur Comm L 221:8–36Google Scholar
  11. 11.
    Wang H, Zhou X-J, Liu Y-Q, Yang H-M, Guo Q-L (2010) Food Addit Contam 27:1261–1265CrossRefGoogle Scholar
  12. 12.
    Cavaliere C, Foglia P, Pastorini E, Samperi R, Lagana A (2006) J Chromatogr, A 1101:69–78CrossRefGoogle Scholar
  13. 13.
    Chen C-Y, Li W-J, Peng K-Y (2005) J Agric Food Chem 53:8474–8480CrossRefGoogle Scholar
  14. 14.
    Aguilera-Luiz MM, Plaza-Bolaños P, Romero-Gonzáles R, Martínez Vidal JL, Garrido Frenich A (2011) Anal Bioanal Chem 399:2863–2875CrossRefGoogle Scholar
  15. 15.
    Wang H, Zhou X-J, Liu Y-Q, Yang H-M, Guo Q-L (2011) J Agric Food Chem 59:3532–3538CrossRefGoogle Scholar
  16. 16.
    Beltrán E, Ibáñez M, Sancho JV, Cortés MA, Yusà V, Hernández F (2011) Food Chem 126:737–744CrossRefGoogle Scholar
  17. 17.
    Herrera-Herrera AV, Asensio-Ramos M, Hernández-Borges J, Rodríguez-Delgado MÁ (2010) Trends Anal Chem 29:728–751CrossRefGoogle Scholar
  18. 18.
    Rezaee M, Yamini Y, Faraji M (2010) J Chromatogr, A 1217:2342–2357CrossRefGoogle Scholar
  19. 19.
    Cruz-Vera M (2010) In: Encyclopedia of analytical chemistry, dispersive liquid-liquid microextraction. Wiley, WeinheimGoogle Scholar
  20. 20.
    Xu X, Su R, Zhao X, Liu Z, Zhang Y, Li D, Li X, Zhang H, Wang Z (2011) Anal Chim Acta 707:92–99CrossRefGoogle Scholar
  21. 21.
    Farajzadeh MA, Djozan D, Reza M, Mogaddam A, Norouzi J (2012) J Sep Sci 35:742–749CrossRefGoogle Scholar
  22. 22.
    Liu X, Zhao A, Zhang A, Liu H, Xiao W, Wang C, Wang X (2011) J Sep Sci 34:1084–1090CrossRefGoogle Scholar
  23. 23.
    Farajzadeh MA, Djozan D, Mogaddam MRA, Bamorowat M (2011) J Sep Sci 34:1309–1316CrossRefGoogle Scholar
  24. 24.
    Cattaneo TMP, Marinoni L, Barzaghi S, Cremonesi K, Monti L (2011) J Chromatogr, A 1218:4738–4745CrossRefGoogle Scholar
  25. 25.
    Vahl M, Jørgensen K (1998) Z Lebensm Unters Forsch 206:243–245CrossRefGoogle Scholar
  26. 26.
    Niessen WMA, Manini P, Andreoli R (2006) Mass Spec Rev 25:881–899CrossRefGoogle Scholar
  27. 27.
    Commission Regulation (EC) 401/2006 (2006) Off J Eur Union L 70:12–(34Google Scholar
  28. 28.
    Berthiller F, Schuhmacher R, Adam G, Krska R (2009) Anal Bioanal Chem 395:1243–1252CrossRefGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2013

Authors and Affiliations

  • Luca Campone
    • 1
  • Anna Lisa Piccinelli
    • 1
    Email author
  • Rita Celano
    • 1
  • Mariateresa Russo
    • 2
  • Luca Rastrelli
    • 1
  1. 1.Dipartimento di FarmaciaUniversità di SalernoFisciano (SA)Italy
  2. 2.Dipartimento di AgrariaUniversità Mediterranea di Reggio CalabriaReggio di CalabriaItaly

Personalised recommendations