Development and Validation of Confirmatory Method for Analysis of Nitrofuran Metabolites in Milk, Honey, Poultry Meat and Fish by Liquid Chromatography-Mass Spectrometry

Open access


In this study we have devoloped and validated a confirmatory analysis method for nitrofuran metabolites, which is in accordance with European Commission Decision 2002/657/EC requirements. Nitrofuran metabolites in honey, milk, poultry meat and fish samples were acidic hydrolised followed by derivatisation with nitrobenzaldehyde and liquid-liquid extracted with ethylacetate. The quantitative and confirmative determination of nitrofuran metbolites was performed by liquid chromatography/electrospray ionisation tandem mass spectrometry (LC/ESI-MS/MS) in the positive ion mode. In-house method validation was performed and reported data of validation (specificity, linearity, recovery, CCα and CCβ). The advantage of this method is that it avoids the use of clean-up by Solid-Phase Extraction (SPE). Furthermore, low levels of nitrofuran metabolites are detectable and quantitatively confirmed at a rapid rate in all samples.

1. Barbosa J., Ferreira S., Pais A.C., Silveria M.I.N. Ramos F. (2011). Nitrofuran in poultry: use, control and residue analysis. In: Hendricks B.P, editor. Agricultural researche updates volume 1. (p 1-50). Hauppauge, New York: Nova Science Publishers, Inc.

2. Commission Decision 1995/1442/EC, 1995 of 26 June 1995, amending of Annexes I, II, III and IV to Regulation (ECC) No 2377/90, laying down a Community Procedure for the establishment of maximum residue limits of veterinary medicinal products in foodstuffs of animal origin. Off. J. Eur. Union, L143;26-30.

3. Commission Decision 2003/181/EC, 13 March 2003, amending decision 2002/657/EC as regards the setting of minimum performance limits (MRPLs) for certain residues in food animal origin, Off. J. Eur. Union, L71/17, 2003.

4. Turkish Food Codex. 2012/23856.

5. European Food Safety Authority (2015). Scientific opinion on nitrofurans and their metabolites in food. EFSA Journal 2015, 13(6): 4140.

6. Harry S.V., George W.H. (1981). Highly specific and sensitive detection method for nitrofurans by thin-layer chromatography. J Chromatogr A, 208 (1), 161-163.

7. Barbosa J., Moura S., Barbosa R., Ramos F. Silveria M.I.N. (2007). Determination of nitrofurans in animal feeds by liquid chromatography-UV photodiode array detection and liquid chromatography-ionspray tandem mass-spectrometry. Anal Chim Acta, 586, 359–365. PMid:17386735

8. McCracken R.J., Kennedy D.G. (1997). Determination of furazolidone in animal feeds chromatography with UV and thermospray mass detection. J Chromatogr A, 771, 349-354.

9. Cooper K.M., Mulder P.P.J., Van Rhijn J.A., Kovacsics L., Mccracken R.J., Young P.B. Kennedy D.G. (2005). Depletion of four nitrofuran antibiotics and their tissue-bound metabolites in porcine tissues and determination using LC-MS/MS and HPLC-UV. Food Addit Contam, 22(5): 406–414. PMid:16019811

10. Rodziewicz L. (2008). Determination of nitrofuran metabolites in milk by liquid chromatography–electrospray ionization tandem mass spectrometry. Journal of Chromatography B, 864 156–160. PMid:18280226

11. Mottier P., Khong S.P., Gremaud E., Richoz J., Delatour T., Goldman T Guy P.A. (2005). Quantitative determination of four nitrofuran metabolites in meat by isotope dilution liquid chromatography–electrospray ionisation–tandem mass spectrometry. J Chromatogr A, 1067 85–91.

12. Szilagyi S., Calle B. (2006). Development and validation of an analytical method for the determination of semicarbazide in fresh egg and in egg powder based on the use of liquid chromatography tandem mass spectrometry Analytica Chimica Acta, 572, 113–120. PMid:17723467

13. Commission Decision 2003/181/EC, 13 March 2003, amending decision 2002/657/EC as regards the setting of minimum performance limits (MRPLs) for certain residues in food animal origin, Off. J. Eur. Union, L71/17, 2003.

Macedonian Veterinary Review

The Journal of the Faculty of Veterinary Medicine-Skopje at the Ss. Cyril and Methodius University in Skopje

Journal Information

CiteScore 2017: 0.32

SCImago Journal Rank (SJR) 2017: 0.195
Source Normalized Impact per Paper (SNIP) 2017: 0.387


All Time Past Year Past 30 Days
Abstract Views 0 0 0
Full Text Views 69 69 17
PDF Downloads 30 30 8