Skip to main content
SpringerLink
Log in

Simultaneous determination of ochratoxin A, mycophenolic acid and fumonisin B2 in meat products

  • Original Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

Here we present a method for simultaneous determination of the fungal metabolites mycophenolic acid, ochratoxin A (OTA) and fumonisin B2 (FB2) in meat products. Extraction was performed with water–acetonitrile, followed by acetone-induced precipitation of salts and proteins. Purification and identification of analytes was performed by mixed-mode reversed-phase anion-exchange chromatography in direct ion-exchange mode, followed by liquid chromatography–tandem mass spectrometry (LC-MS/MS) detection. Quantification was based on isotope dilution with fully 13C-labelled FB2 and OTA, and matrix-spiked calibration curves. Fermented sausages inoculated with an OTA- and FB2-producing strain of Aspergillus niger were analysed, but no analytes were detected. Analysis of 22 retail products showed one Parma meat with a very high level of OTA contamination (56–158 μg/kg) that clearly exceeded the Italian regulatory limit of 1 μg/kg. This sample and uninfected control samples were subsequently reanalysed, and the high OTA content was verified by two other techniques: (i) LC–time-of-flight MS confirmed the accurate mass as well as chlorine isotope pattern; and (ii) sample methylation in methanol–BF3 and subsequent LC-MS/MS provided indirect confirmation by detection of the OTA methyl ester. In the contaminated Parma ham, the high OTA level most likely originated from growth of Penicillium nordicum on the meat.

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

Access this article

Log in via an institution

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

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2

Similar content being viewed by others

References

  1. Sorensen LM, Nielsen KF, Jacobsen T, Koch AG, Nielsen PV, Frisvad JC (2008) J Chromatogr A 1205:103–108

    Article  CAS  Google Scholar 

  2. Iacumin L, Chiesa L, Boscolo D, Manzano M, Cantoni C, Orlic S, Comi G (2009) Food Microbiol 26:65–70

    Article  CAS  Google Scholar 

  3. Spotti E, Cacchioli C, Colla F, Beatrisotti M, Zanardi S (1999) Industria Conserve 74:113–124

    Google Scholar 

  4. Spotti E, Chiavaro E, Pari E, Busolli C (2001) Industria Conserve 76:167–183

    Google Scholar 

  5. Larsen TO, Svendsen A, Smedsgaard J (2001) Appl Environ Microbiol 67:3630–3635

    Article  CAS  Google Scholar 

  6. Gareis M, Scheuer R (2000) Arch Lebensmittelhyg 51:102–104

    CAS  Google Scholar 

  7. Dall'Asta C, Galaverna G, Bertuzzi T, Moseriti A, Pietri A, Dossena A, Marchelli R (2010) Food Chem 120:978–983

    Article  Google Scholar 

  8. Monaci L, Palmisano F, Matrella R, Tantillo G (2005) J Chromatogr A 1090:184–187

    Article  CAS  Google Scholar 

  9. Toscani T, Moseriti A, Dossena A, Asta CD, Simoncini N, Virgili R (2007) J Chromatogr B Analyt Technol Biomed Life Sci 855:242–248

    Article  CAS  Google Scholar 

  10. Jørgensen K, Petersen A (2002) Food Addit Contam 19:562–567

    Article  Google Scholar 

  11. Andersen SJ (1995) J Food Prot 58:426–429

    Google Scholar 

  12. Asefa DT, Gjerde RO, Sidhu MS, Langsrud S, Kure CF, Nesbakken T, Skaar I (2009) Int J Food Microbiol 128:435–439

    Article  CAS  Google Scholar 

  13. Battilani P et al (2007) J Food Prot 70:975–980

    Google Scholar 

  14. Peintner U, Geiger J, Pöder R (2000) J Food Prot 63:1399–1403

    CAS  Google Scholar 

  15. Tabuc C, Bailly JD, Bailly S, Querin A, Guerre P (2004) Rev Med Vet 155:287–291

    Google Scholar 

  16. Chiavaro E, Lepiani A, Colla F, Bettoni P, Pari E, Spotti E (2002) Food Addit Contam 19:575–581

    Article  CAS  Google Scholar 

  17. Jimenez AM, de Cerain AL, Gonzalez-Penas E, Bello J (2001) Food Addit Contam 18:559–563

    CAS  Google Scholar 

  18. Spotti E, Chiavaro E, Lepiani A, Colla F (2001) Industria Conserve 76:341–354

    Google Scholar 

  19. Commission of the European Communities (2006) EC No 1881/2006 of 19 December 2006 setting maximum levels for certain contaminants in foodstuffs

  20. Food and Agriculture Organization of the United Nations (2003) Worldwide regulations for mycotoxins in food and feed in 2003, FAO Food and Nutrition Paper 80

  21. Bentley R (2000) Chem Rev 100:3801–3825

    Article  CAS  Google Scholar 

  22. Huerta T, Sanchis V, Hernandez J, Hernandez E (1987) Microbiol Aliments Nutr 5:247–252

    Google Scholar 

  23. Leistner L, Ayres JC (1967) Die Fleischwirtschaft 47:1320–1326

    Google Scholar 

  24. Mizáková A, Pipová M, Turek P (2002) Czech J Food Sci 20:89–94

    Google Scholar 

  25. Nunez F, Rodriguez MM, Bermudez ME, Cordoba JJ, Asensio MA (1996) Int J Food Microbiol 32:185–197

    Article  CAS  Google Scholar 

  26. Rojas FJ, Jodral M, Gosalvez F, Pozo R (1991) Int J Food Microbiol 13:249–256

    Article  CAS  Google Scholar 

  27. Frisvad JC, Smedsgaard J, Samson RA, Larsen TO, Thrane U (2007) J Agric Food Chem 55:9727–9732

    Article  CAS  Google Scholar 

  28. Månsson M, Klejnstrup ML, Phipps RK, Nielsen KF, Frisvad JC, Godtfredsen CH, Larsen TO (2010) J Agric Food Chem 58:949–953

    Article  Google Scholar 

  29. Mogensen JM, Frisvad JC, Thrane U, Nielsen KF (2010) J Agric Food Chem 58:954–958

    Article  CAS  Google Scholar 

  30. Noonim P, Mahakarnchanakul W, Nielsen KF, Frisvad JC, Samson RA (2009) Food Addit Contam 26:94–100

    Article  CAS  Google Scholar 

  31. Abarca ML, Bragulat MR, Castellá G, Cabañes FJ (1994) Appl Environ Microbiol 60:2650–2652

    CAS  Google Scholar 

  32. Accensi F, Abarca ML, Cano J, Figuera L, Cabanes FJ (2001) Antonie Leeuwenhoek 79:365–370

    Article  CAS  Google Scholar 

  33. Magnoli C, Violante M, Combina M, Palacio G, Dalcero A (2003) Lett Appl Microbiol 37:179–184

    Article  CAS  Google Scholar 

  34. Logrieco A, Ferracane R, Haidukowsky M, Cozzi G, Visconti A, Ritieni A (2009) Food Addit Contam A Chem Anal Control Expo Risk Assess 26:1495–1500

    CAS  Google Scholar 

  35. Gelderblom WCA, Cawood ME, Snyman SD, Vleggaar R, Marasas WFO (1993) Food Chem Toxicol 31:407–414

    Article  CAS  Google Scholar 

  36. Gutleb AC, Morrison E, Murk AJ (2002) Environ Toxicol Pharmacol 11:309–320

    Article  CAS  Google Scholar 

  37. Chu FS, Li GY (1994) Appl Environ Microbiol 60:847–852

    CAS  Google Scholar 

  38. Marasas WFO, Jaskiewicz K, Venter FS, Vanschalkwyk DJ (1988) S Afr Med J 74:110–114

    CAS  Google Scholar 

  39. Sydenham EW, Thiel PG, Marasas WFO, Shephard GS, Vanschalkwyk DJ, Koch KR (1990) J Agric Food Chem 38:1900–1903

    Article  CAS  Google Scholar 

  40. Yoshizawa T, Yamashita A, Luo Y (1994) Appl Environ Microbiol 60:1626–1629

    CAS  Google Scholar 

  41. Losito I, Monaci L, Palmisano F, Tantillo G (2004) Rapid Commun Mass Spectrom 18:1965–1971

    Article  CAS  Google Scholar 

  42. Månsson M, Phipps RK, Gram L, Munro MH, Larsen TO, Nielsen KF (2010) J Nat Prod 73:1126–1132

    Article  Google Scholar 

  43. Mogensen JM, Larsen TO, Nielsen KF (2010) J Agric Food Chem 58:4853–4857

    Article  CAS  Google Scholar 

  44. Nielsen KF, Smedsgaard J (2003) J Chromatogr A 1002:111–136

    Article  CAS  Google Scholar 

  45. Valenta H (1998) J Chromatogr A 815:75–92

    Article  CAS  Google Scholar 

  46. Commission of the European Communities (1996) Council Directive 96/23/EC of 29 April 1996 on measures to monitor certain substances and residues thereof in live animals and animal products

  47. Commission of the European Communities (2002) Commission Decision 2002/657/EC of 12 August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results

  48. Paepens C, De Saeger S, Van Poucke C, Dumoulin F, Van Calenbergh S, Van Peteghem C (2005) Rapid Commun Mass Spectrom 19:2021–2029

    Article  CAS  Google Scholar 

  49. Muscarella M, Magroa SL, Nardiello D, Palermo C, Centonze D (2008) J Chromatogr A 1203:88–93

    Article  CAS  Google Scholar 

  50. Spanjer MC, Rensen PM, Scholten JM (2008) Food Addit Contam 25:472–489

    Article  CAS  Google Scholar 

  51. Krska R, Welzig E, Boudra H (2007) Anim Feed Sci Technol 137:241–264

    Article  CAS  Google Scholar 

  52. Annesley TM (2003) Clin Chem 49:1041–1044

    Article  CAS  Google Scholar 

  53. Klotzel M, Gutsche B, Lauber U, Humpf HU (2005) J Agric Food Chem 53:8904–8910

    Article  Google Scholar 

  54. Sospedra I, Blesa J, Soriano JM, Manes J (2010) J Chromatogr A 1217:1437–1440

    Article  CAS  Google Scholar 

  55. Nielsen KF, Graefenhan T, Zafari D, Thrane U (2005) J Agric Food Chem 53:8190–8196

    Article  CAS  Google Scholar 

  56. Joint FAO/WHO Expert Committee on Food Additives (2007) Evaluation of certain food additives and contaminants (sixty-eighth report of the Joint FAO/WHO Expert Committee on Food Additives)

Download references

Acknowledgements

We are thankful for the supply of raw sausages from the Danish Meat Research Institute. This project was supported by the Danish Meat Association, the Centre for Advanced Food Studies, and the Danish Food Industry Agency (grant 3304-FVEP-07-730-01).

Author information

Authors and Affiliations

  1. Department of Systems Biology, Technical University of Denmark, Building 221, 2800, Lyngby, Denmark

    Louise Marie Sørensen, Jesper Mogensen & Kristian Fog Nielsen

  2. Department of Food Science, University of Copenhagen, Rolighedsvej 30, 1958, Frederiksberg, Copenhagen, Denmark

    Louise Marie Sørensen

Authors
  1. Louise Marie Sørensen
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Jesper Mogensen
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Kristian Fog Nielsen
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Kristian Fog Nielsen.

Electronic supplementary material

Below is the link to the electronic supplementary material.

ESM 1

(PDF 538 kb)

Rights and permissions

Reprints and permissions

About this article

Cite this article

Sørensen, L.M., Mogensen, J. & Nielsen, K.F. Simultaneous determination of ochratoxin A, mycophenolic acid and fumonisin B2 in meat products. Anal Bioanal Chem 398, 1535–1542 (2010). https://doi.org/10.1007/s00216-010-4059-z

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-010-4059-z

Keywords

Search

Navigation