A liquid chromatography-ultraviolet detection method for the determination of florfenicol (FF) and thiamphenicol (TAP) in feeds is presented. The method comprises the extraction of analytes from the matrix with a mixture of methanol and acetonitrile, drying of the extract, and its dissolution in phosphate buffer. The analysis was performed with a gradient programme of the mobile phase composed of acetonitrile and buffer (pH = 7.3) on a Zorbax Eclipse Plus C18 (150 × 4.6 mm, 5 μm) analytical column with UV (λ = 220 nm) detection. The analytical procedure has been successfully adopted and validated for quantitative determination of florfenicol and thiamphenicol in feed samples. Sensitivity, specificity, linearity, repeatability, and intralaboratory reproducibility were included in the validation. The mean recovery of amphenicols was 93.5% within the working range of 50-4000 mg/kg. Simultaneous determination of chloramphenicol, which is banned in the feed, was also included within the same procedure of FF and TAP stability studies. Storing the medicated feed at room temperature for up to one month decreased concentration in the investigated drugs even by 45%. These findings are relevant to successful provision of therapy to animals.
If the inline PDF is not rendering correctly, you can download the PDF file here.
1. Andrée S. Jira W. Schwind K.H. Wagner H. Schwägele F.: Chemical safety of meat and meat products. Meat Sci 2010 86 38-48.
2. Bilandžić N. Varenina I. Solomun Kolanović B.: Control of chloramphenicol in samples of meat meat products and fish. Meso 2011 13 192-196.
3. Boscher A. Guignard C. Pellet T. Hoffmann L. Bohn T.: Development of a multi-class method for the quantification of veterinary drug residues in feeds by liquid chromatographytandem mass spectrometry. J Chromatogr A 2010 1217 6394-6404.
4. Commission Decision 2001/1322/EC of 29 June 2001 Amending Annexes I and III to Council Regulation (EEC) No. 2377/90 laying down a community procedure for the establishment of maximum residue limits of veterinary medicinal products in foodstuffs of animal origin. OJL177/52 30.6.2001.
5. Commission Decision 2002/657/EC implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. OJ L. 221 17.8.2002 pp. 16-17.
6. Commission Decision 2003/181/EC of 13 March 2003 on amending Decision 2002/657/EC as regards of minimum required performance limits (MRPLs) for certain residues in food of animal origin. OJ L71 15.03.2003 pp. 17-18.
7. Commission Regulation (EC) No. 1805/2006 of 7 December 2006 Amending Annex I to Council Regulation (EEC) No 2377/90 laying down a community procedure for the establishment of maximum residue limits of veterinary medicinal products in foodstuffs of animal origin as regards thiamphenicol fenvalerate and meloxicam. OJ L 343 8.12.2006 pp. 66-68.
8. Council Directive 90/167/EEC laying down the conditions governing the preparation placing on the market and use of medicated feeds in the Community. OJ L 92 07.04.1990 pp. 42-48.
9. Dang P.K. Degand G. Douny C. Ton V.D. Maghuin-Rogister G. Scippo M.L.: Optimisation of a new two-plate screening method for the detection of antibiotic residues in meat. Int J Food Sci Tech 2011 46 2070-2076 doi:10.1111/j.1365-2621.2011.02718.x
10. Falagas M.E. Grammatikos A.P. Michalopoulos A.: Potential of old-generation antibiotics to address current need for new antibiotics. Expert Rev Anti Infect Therapy 2008 6 593-600. doi:10.1586/1478722.214.171.1243. PMID 18847400.
11. Franje C.A. Changb S.K. Shyua C.L. Davisc J.L. Leea Y.W.: Differential heat stability of amphenicols characterized by structural degradation mass spectrometry and antimicrobial activity. J Pharmaceut Biomed 2010 53 869-877.
12. Fuchs F.D.: "Tetraciclinas e cloranfenicol". In: Farmacologia clínica: fundamentos da terapêutica racional. Edited by Fuchs F.D. Wannmacher L. Ferreira M.B. Guanabara Koogan Rio de Janeiro 2004. p. 375.
13. Hayes J.M.: Determination of florfenicol in fish feed by liquid chromatography. J AOAC Int 2005 88 1777-1783.
14. Hayes J.M. Gilewicz R. Freehauf K. Fetter M.: Assay of florfenicol in swine feed: interlaboratory study. J AOAC Int 2009 92 340-347.
15. Huet A.C. Fodey T. Haughey S.A. Weigel S. Elliott C. Delahaut P.: Advances in biosensor-based analysis for antimicrobial residues in foods. Trend Anal Chem 2010 29 1281-1294.
16. Luo P.J. Cao X.Y. Wang Z.H. Jiang H.Y. Zhang S.X. Chen X. Wang J.P. Feng C.M. Shen J.Z.: Development of an enzyme-linked immunosorbent assay for the detection of florfenicol in fish feed. Food Agr Immunol 2009 20 57-65.
17. Luo P.J. Jiang W.X. Chen X. Shen J.Z. Wu Y.N.: Technical note: development of an enzyme-linked immunosorbent assay for the determination of florfenicol and thiamphenicol in swine feed. J Anim Sci 2011 89 3612-3616.
18. Patyra E. Kowalczyk E. Kwiatek K.: Determination of chlorotetracycline and doxycycline in medicated feedingstuffs by liquid chromatography. Bull Vet Inst Pulawy 2012 56 329-333.
19. Pietroń W.J. Cybulski W. Krasucka D. Mitura A. Kos K. Antczak M.: Determination of five sulphonamides in medicated feedingstuffs by liquid chromatograph with ultraviolet detection. Bull Vet Inst Pulawy 2013 57 545-552
20. Pouliquen H. Morvan M.L.: Determination of florfenicol in freshwater sediments and bryophyte fontinalis antipyretica by HPLC with fluorescence detection. Chromatographia 2005 62 225-231.
21. Regulation (EC) No 882/2004 of the European Parliament and of the Council of 29 April 2004. On official controls performed to ensure the verification of compliance with feed and food law animal health and animal welfare rules.
22. Rich M. Ritterhoff R. Hoffmann R.: A fatal case of aplastic anemia following chloramphenicol (chloromycetin) therapy. Ann Int Med 1950 33 1459-1467.
23. Riviere J.E. Papich M.G. Veterinary Pharmacology and Therapeutics. Wiley-BlackWell Hong Kong 2009.
24. Shen J.Z. Xia X. Jiang H. Li C. Li J. Li X. Ding S.: Determination of chloramphenicol thiamphenicol florfenicol and florfenicol amine in poultry and porcine muscle and liver by gas chromatography-negative chemical ionization mass spectrometry. J Chromatogr B 2009 877 1523-1529.
25. Shinoda N. Kojima F. Sugiura K.J.: Residuals. Simultaneous determination of residues of chloramphenicol and florfenicol in animal feed by liquid chromatography tandem mass spectrometry. J Residuals Sci Tech 2011 8 125-129.
26. Syriopoulou V.P. Harding A.L. Goldmann D.A. Smith AL.: In vitro antibacterial activity of fluorinated analogs of chloramphenicol and thiamphenicol. Antimicrob Agents Chemother 1981 19 294-297.
27. Sniegocki T. Posyniak A. Gbylik-Sikorska A. Zmudzki J.: Determination of chloramphenicol in milk using a QuEChERSbased on liquid chromatography tandem mass spectrometry method. Anal Lett 2014 47 568-578.
28. The Annual Report of The Rapid Alert System for Food and Feed (Rapid Alert System for Food and Feed RASFF 2007. doi:10.2772/63727
29. The Annual Report of The Rapid Alert System for Food and Feed (Rapid Alert System for Food and Feed RASFF 2013. doi:10.2772/33031.
30. Vega M.H. Jara E.T. Aranda M.B.: Monitoring the dose of florfenicol in medicated salmon feed by planar chromatography (HPTLC) Jap J Planar Chromat 2006 19 204-207.
31. Vue C. Schmidt L. J. Stehly G.R. Gingerich W.H.: Liquid chromatographic determination of florefnicol in the plasma of multiple species of fish. J Chromatogr B 780 2002 111-117.
32. Wen L.L. Ren J.L. Maw R.L.: Supercritical fluid extraction in situ derivatization for simultaneous determination of chloramphenicol florfenicol and thiamphenicol in shrimp. Food Chem 2010 121 797-802.