Introduction: The article presents a rapid and simple analytical procedure for determination of four tetracyclines (oxytetracycline, tetracycline, chlortetracycline, and doxycycline) in animal medicated feedingstuffs. Material and Methods: Two-gramme samples were extracted by a Na2EDTA-McIlvaine buffer (pH 4)/methanol mixtures (40/60, v/v). The determination was achieved by liquid chromatography using a Zorbax Eclipse XDB C18 analytical column with mass spectrometer detection (LC-MS). Results: Recoveries of the antibiotics from spiked feed samples ranged from 78.2% to 113.5%. The LOD and LOQ for tetracyclines in feeds ranged from 2.8 to 4.2 and from 4.3 to 5.7 mg/kg, respectively. Conclusion: The method was successfully validated and proved to be efficient, precise, and useful for quantification of tetracyclines in medicated feedingstuffs.
If the inline PDF is not rendering correctly, you can download the PDF file here.
1. Andersen W.C. Roybal J.E. Gonzales S.A. Turnipseed S.B. Pfenning A.P. Kuck L.R.: Determination of tetracycline residues in shrimp and whole milk using liquid chromatography with ultraviolet detection and residue confirmation by mass spectrometry. Anal Chim Acta 2004 529 145-150.
2. Blanchflower W.J. McCracken R.J. Rice D.A.: Determination of chlortetracycline residues in tissues using high-performance liquid chromatography with fluorescence detection. Analyst 1989 114 421-423.
3. Boscher A. Guignard C. Pellet T. Hoffman L. Bohn T.: Development of a multi-class method for the quantification of veterinary drug residue in feedingstuffs by liquid chromatography-tandem mass spectrometry. J Chromatogr A 2010 1217 6394-6404.
4. Caballero R.D. Torre-Lapasio R. Garcia-Alvarez-Coque M.C. Ramis-Ramos G.: Rapid liquid determination of tetracyclines in animal feeds using a surfactant solution as mobile phase. Anal Lett 2002 35 687-705.
5. Carrasco-Pancorbo A. Casado-Terrone S. Segura-Carretero A. Fernández-Gutiérrez A.: A reversed-phase high-performance liquid chromatography coupled to ultraviolet and electrospray time-of-flight mass spectrometry on-line detection for the separation of eight tetracyclines in honey samples. J Chromatogr A 2008 1195 107-116.
6. Chafer-Pericas C. Maquieira A. Puchades R. Miralles J. Moreno A.: Multiresidue determination of antibiotics in feed and fish samples for food safety evaluation. Comparison of immunoassay vs LC-MS-MS Food Control 2011 22 993-999.
7. Cherlet M. Schelkens M. Croubels S. De Backer P.: Quantitative multi-residue analysis of tetracyclines and their 4-epimers in pig tissues by high-performance liquid chromatography combined with positive-ion electrospray ionization mass spectrometry. Anal Chim Acta 2003 492 199-213.
8. Fiori J. Grassigli G. Filippi P. Gotti R. Cavrini V.: HPLCDAD and LC-MS analysis of doxycycline and related impurities in doxipin mix a medicated premix for incorporation in medicated feedstuffs. J Pharma Biomed Anal 2005 37 979-985.
9. Gafner J.L.: Identification and semiquantitative estimation of antibiotics added to complete feeds premixes and concentrates. J AOAC Int 1999 82 1-8.
10. Guo L. Chen Y. Zhang L. Yang W. He P.: Development and validation of a liquid chromatographic/tandem mass spectrometric method for determination of chlortetracyclines oxytetracyclines tetetracyclines and doxycyclines in animal feeds. J AOAC Int 2012 95 1010-1015.
11. Injac R. Mlinaric A. Djorjevic-Milic V. Karljikovic-Rajic K. Strukelj B.: Optimal conditions for determination of zinc bacitracin polymyxin B oxytetracycline and sulfacetamide in animal feed by micellar electrokinetic capillary chromatography. Food Addit Cont 2008 4 424-431.
12. Kaklamanos G. Vincent U. von Holst C.: Analysis of antimicrobial agents in pig feed by liquid chromatography coupled to orbitrap mass spectrometry. J Chromatogr A 2013 1293 60-74.
13. Khan N.H. Roets E. Hoogmartens J. Vanderhaeghe H.: Quantitative analysis of oxytetracycline and related substances by high-performance liquid chromatography. J Chromatogr A 1987 405 229-245.
14. Ma T.Y. Vickroy T.W. Shien J.H. Chou C.C.: Improved nonaqueous capillary electrophoresis for tetracyclines at subparts per billion level. Electrophoresis 2012 33 1679-1682.
15. Markaksis P.K.: Determination of tetracyclines in animal feeds in the presence of other drugs by thin-layer chromatography and microbiological method. J AOAC Int 1996 79 375-379.
16. Martinez E. Shimoda W.: Liquid chromatographic determination of tetracycline residue in animal feeds. J Assoc Off Anal Chim 1987 71 477-480.
17. Martinez E. Shimoda W.: Liquid chromatographic determination of epimerization of chlortetracycline residue to 4-epi-chlorotetracycline residue in animal feed using McIlvain’s buffer as extractant. J Assoc Off Anal Chem 1989 72 848-850.
18. Mulders E.J Van De Lagemaat D.: Determination of residues of tetracycline antibiotics in animal tissues by high-performance liquid chromatography. J Pharm Biomed Anal 1992 7 1829-1835.
19. Oka H. Ito Y. Matsumoto H.: Chromatographic analysis of tetracycline antibiotics in foods. J Chromatogr A 2000 882 109-133.
20. Patyra E. Kowalczyk E. Kwiatek K.: Development and validation method for the determination of delected tetracylines in animal medicated feedingstuffs with the use of micellar liquid chromatography. Anal Bioanal Chem 2013 405 6799-6806.
21. Schnappinger D. Hillen W.: Tetracyclines: antibiotic action uptake and resistance mechanisms. Arch Microbiol 1996 165 359-369.
22. Tong J. Rao Q. K. Jiang Z. Ding S.: Simultaneous determination of five tetracycline and macrolide antibiotics in feed using HPCE. J Sep Sci 2009 32 4254-4260.
23. Udalova A.Y. Dmitrienko S.G. Apyari V.V.: Methods for the separation preconcentration and determination of tetracycline antibiotics. J Anal Chem 2015 70 661-676.
24. Vinas P. Balsalobre N. Lopez-Erroz C. Hernandez-Cordoba M.: Liquid chromatography with ultraviolet absorbance detection for the analysis of tetracycline residue in honey. J Chromatogr A 2004 1022 125-129.
25. Walsh J. Walker L.V. Webber J.J.: Determination of tetracyclines in bovine and porcine muscle by high-performance liquid chromatography using solid-phase extraction. J Chromatogr A 1992 596 211-216.