Study on the method performances for screening and confirmatory analysis of aflatoxin M1 in raw milk according to the mycotoxin regulative requirements

Authors

  • Elizabeta Dimitrieska-Stojkovik Faculty for Veterinary Medicine, Food Institute Ss. Cyril and Methodius University Skopje, Republic of Macedonia
  • Gordana Ilievska Faculty for Veterinary Medicine, Food Institute Ss. Cyril and Methodius University Skopje, Republic of Macedonia
  • Biljana Stojanovska-Dimzoska Faculty for Veterinary Medicine, Food Institute Ss. Cyril and Methodius University Skopje, Republic of Macedonia
  • Risto Uzunov Faculty for Veterinary Medicine, Food Institute Ss. Cyril and Methodius University Skopje, Republic of Macedonia
  • Zehra Hajrulai-Musliu Faculty for Veterinary Medicine, Food Institute Ss. Cyril and Methodius University Skopje, Republic of Macedonia

DOI:

https://doi.org/10.20450/mjcce.2014.486

Keywords:

Aflatoxin M1, raw milk, Immunoenzimatic assay, HPLC-FD, 657/2002/EC,

Abstract

Screening and confirmatory methods for Aflatoxin M1 (AFM1) analysis were optimized and studied regarding the European Decision 2002/657/EC requirements. The recoveries of AFM1 from the spiked samples at levels between 0.025 and 0.075 µg kg-1 were 99.6-110.3 % with obtained precision 10.5-13.4 %, confirming the immunochemical method precision and reliability for intensive surveillance studies. According to the regulatory requirements, for confirmation of the obtained positives from the screening, the reference high-performance liquid chromatographic method was evaluated in reference to the performance criteria. The obtained between-day recovery was in the range 67.2-72.8 %, and the precision range 5.4-9.1 %. 205 positives from the screening were subjected to confirmatory analysis. The comparison of the data obtained from the immunoassay and chromatographic method (R2=0.764) revealed a slight overestimation of the screening method, but no cases of false-negative determinations occurred.

Author Biography

Elizabeta Dimitrieska-Stojkovik, Faculty for Veterinary Medicine, Food Institute Ss. Cyril and Methodius University Skopje, Republic of Macedonia

Head of the laboratory for rezidues and contaminants

 

References

P. B. Wangikar, P. Dwivedi, N. Sinha, A. K. Sharma, A. G. Telang, Effects of aflatoxin B1 on embryo fetal development in rabbits, Food Chem. Toxicol., 43, 607–615 (2005).

J. H. Williams, D. T. Phillips, P. E. Jolly, J. K. Sttiles, C. M. Jolly, D. Aggaewal, Human aflatoxicosis in developing counties: A review of toxicology, exposure, potential health consequences and intervention, Am. J. Clin. Nutr., 80, 1106–1122 (2004).

International Agency for Research on Cancer (IARC), IARC Monographs on the evaluation of carcinogenic risks to human, IARC Lyon, France, Vol. 56, 1993, 246–362.

I. Bakirci, A study on the occurrence of Aflatoxin M1 in milk and milk products produced in Van province of Turkey, Food Control, 12 47–51 (2001).

A. Govaris, V. Roussi, P. A. Koidis, N. A. Botsoglou, Distribution and stability of Aflatoxin M1 during pro-duction and storage of yogurt, Food Addit. Contam., 19 (11) 1043–1050 (2002).

International Agency for Research on Cancer (IARC), IARC Monographs on the evaluation of carcinogenic risks to human, IARC Lyon, France, Vol. 6, 2002, 171–176.

European Parliament and Council Directive 96/23/EC of 23 May 1996, Off. J. European Union, L77, 10–16 (1996).

European Commission Regulation No. 1881/2006/EC of 19 December 2006, Off. J. European Union, L364, 5–24 (2006).

EN ISO 14675:2003 – Milk and milk products – Guidelines for a standardized description of competitive enzyme immunoassays – Determination of Aflatoxin M1 content, European Committee for Standardization, 2003.

P. Gallo, A. Salzillo, C. Rossini, V. Urbani, L. Serpe, Aflatoxin M1 determination in milk: Method validation and contamination levels in samples from Southern Italy, Ital. J. Food Sci., 18(3) 251–259 (2006).

A. C. Manneta, L. di Giuseppe, M. Giammarco, I. Fusaro, A. Simonella, A. Gramenzi, A. Formigoni, High–performance liquid chromatography with post-column derivatization and fluorescence detection for sensitive determination of aflatoxin M1 in milk and cheese, J. Chromatogr. A, 1083, 219–222 (2005).

M. Muscarella, S. Lo Magro, C. Palermo, D. Centonze, Validation according to European Commission Decision 2002/657/EC of a confirmatory method for aflatoxin M1 in milk based on immunoaffinity columns and high performance liquid chromatography with fluorescence detection, Anal. Chim. Acta, 594, 257–264 (2007).

V.A. Alonso, M.P. Monge, A. Larriestra, A.M. Dalcero, L.R. Cavaglieri and S.M. Chiacchiera, Naturally occurring aflatoxin M1 in bulk milk from farm cooling tanks in Argentina, Food Addit. Contam., 27 (3), 373-379 (2010).

H. Wang, X.J. Zhou, Y.Q. Liu, H.M. Yang, Q.L.Guo, Determination of aflatoxin M1 in milk by triple quadrupole liquid chromatography-tandem mass spec-trometry, Food Addit. Contam., 27 (9), 1261-1265 (2010).

E. Beltrán, M. Ibáñez, J.V. Sancho, M.Á. Cortés and V. Yusà, UHPLC-MS/MS highly sensitive determination of aflatoxins, the aflatoxin metabolite M1 in baby food and milk, Food Chem., 126, 737-744 (2011).

B. Škrbić, J. Živančev, I. Antić, M. Godula, Levels of aflatoxin M1 in different types of milk collected in Serbia: Assessment of human and animal exposure, Food Control, 40, 113-119 (2014).

K. Thirumala-Devi, M. A. Mayo, A. J. Hall, Develop-ment and application of an indirect competitive en-zyme-linked immunoassay for aflatoxin M1 in milk and milk-based confectionery, J. Agric. Food Chem., 50 (4) 933–937 (2002).

M. Magliulo, M. Mirasoli, P. Simoni, R. Ielli, O. Portanti, A. Roda, Development and validation of an ultrasensitive chemiluminiscent anzyme immunoassay for Aflatoxin M1 in milk, J. Agric. Food Chem., 53 (9) 3300–3305 (2005).

P. Rosi, A. Borsari, G. Lasi, S. Lodi, A. Galanti, A. Fava, S. Girotti, E. Ferri, Aflatoxin M1 in milk: Reliability of the immunoenzymatic assay, Int. Dairy J., 17, 429–435 (2007).

L. Anfossi, M. Calderara, C. Baggiani, C. Giovannoli, E. Arletti, G. Giraudi, Development and Application of Solvent-free Extraction for the Detection of Aflatoxin M1 in Diary Products by Enzyme Immunoassays, J. Agric. Food Chem., 56 1852–1857 (2008).

R. Rubio, M. I. Berruga, M. Román, A. Molina, Evaluation of immunoenzymatic methods for the detection of aflatoxin M1 in ewe’s milk, Food Control, 20, 1049–1052 (2009).

D. Guan, P. Li, Y. Cui, Q. Zhang, W. Zhang, A competitive immunoassay with a surrogate calibrator curve for aflatoxin M1 in milk, Anal. Chim. Acta, 703, 64–69 (2011).

EN ISO 14501:2007 – Milk and milk powder – Deter-mination of Aflatoxin M1 content – Clean-up by immunoaffinity chromatography and determination by high-performance liquid chromatography, European Committee for Standardization, 2003.

European Commission Regulation (EC) No 401/2006 of 23 February 2006, Off. J. European Union L70, 12–34 (2006).

European Commission Decision 2002/657/EC of 12 April 2002, Off. J. European Union L 221, 8–36 (2002).

E. E. Kim, D. H. Shon, D. Ryu, J. W. Park, H. J. Hwang, Y. B. Kim, Occurrence of aflatoxin M1 in Korean dairy products determined by ELISA and HPLC, Food Addit. Contam., 17, 59–64 (2000).

J. C. Miler and J. N. Miler, Statistics for Analytical Chemistry, 3rd edition, Ellis Horwood Ltd. Chichester, West Sussex, 1994.

EURACHEM/CITAC Guide cg 4, in: S. L. R. Ellison, M. Rosslein, A. Williams (Eds.). Quantifying Uncertainty in Analytical Measurement, Second ed. 2000.

N. Bilandžić, I. Varenina, B. Solomun, Aflatoxin M1 in raw milk in Croatia, Food Control, 21, 1379–1281 (2010).

J. Kos, J. Lević, O. Ðuragić, B. Kokić, I. Miladinović, Occurrence and estimation of aflatoxin M1 exposure in milk in Serbia, Food Control, 38, 41–46 (2014).

Community Reference Laboratories Residues (CRLs), Guidelines for the validation of screening methods for residues of veterinary medicines.

http://crl.fougeres.anses.fr/publicdoc/Guideline_Validation_Screening_en.pdf, 20th January 2010 (accessed 14.01.2014).

International Standards Organization ISO 8258: Shewhart Control Charts, ISO, Geneva, Switzerland, 1991.

D. N. Mortimer, J. Gilbert, M. J. Shepherd, Rapid and highly sensitive analysis of aflatoxin M1 in liquid and powdered milks using an affinity column cleanup, J. Chromatogr A 407 (1987).

Metodi chimici di analisi per l`esame degli alimenti (Chemical methods of analysis for the examination of foods), ISTISAN Report 96/34, ISSN 1123–3177, 218–219 (1996).

M. Thompson, Recent trends in inter-laboratory preci-sion at ppb and sub-ppb concentrations in relation to fitness for purpose criteria in proficiency testing, Analyst, 125, 385–386 (2000).

G. Calaresu, P. Piras, G. Carta, R. Galarini, G. Chessa, Estimation of measurement of uncertainty for the determination of aflatoxin M1 in milk using immunoaffinity clean-up procedures, Accred. Qual. Assur. 11, 10–16 (2006).

E. Malissova, A. Tsakalof, I. S. Arvanitoyannis, A. Katsafliaka, A. Katsioulis, P. Tserkezou, M. Koureas, A. Govaris, C. Hadjichristodoulou, Monitoring Aflatoxin M1 levels in ewe’s and goat’s milk in Thessaly, Greece; potential risk factors under organic and conventional production schemes, Food Control, 34, 241–248 (2013).

Downloads

Published

2014-12-01

How to Cite

Dimitrieska-Stojkovik, E., Ilievska, G., Stojanovska-Dimzoska, B., Uzunov, R., & Hajrulai-Musliu, Z. (2014). Study on the method performances for screening and confirmatory analysis of aflatoxin M1 in raw milk according to the mycotoxin regulative requirements. Macedonian Journal of Chemistry and Chemical Engineering, 33(2), 217–226. https://doi.org/10.20450/mjcce.2014.486

Issue

Section

Food Chemistry

Most read articles by the same author(s)