Determinaton of enrofloxacin and ciprofloxacin in albumin and freeze-dried-eggs by liquid chromatography with fluorescence detection

Open access


The study presents a method for determination of enrofloxacin and ciprofloxacin in albumin and freeze-dried-eggs with the use of liquid chromatography with fluorescence detection. The procedure enables a simple isolation of fluoroquinolones from albumin based on extraction with acetonitrile, and from freeze-dried-eggs with acetonitrile under alkaline conditions. The samples have been analysed on ultracarb C8 liquid chromatography column. The gradient elution programmes consisted of the mixture of 0.03 M phosphoric acid with 0.002 M sodium 1-heptanesulfonate monohydrate and acetonitrile. The method has been validated according to requirements of the European Decision 2002/657/EC. Recoveries ranged from 78% to 83% for spiked freeze-dried-eggs and from 89% to 91% for albumin. The developed method can be applied for determination and confirmation of enrofloxacin and ciprofloxacin in albumin and freeze-dried-eggs.

1. Blondeau J.M.: Fluoroquinolones: mechanism of action, classification, and development of resistance. Surv Ophthalmol 2004, 49, 73-78.

2. Commission Decision 2002/657/EC of August 2002 implementing Council Directive 96/23/EC concerning the performance of analytical methods and the interpretation of results. Official Publications of the European Communities 2002, L 221, 8-36.

3. Commission Regulation (EU) No 37/2010 of 22 December 2009 on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin, L15, 1-72.

4. Chu. P., Wang R., Chu H.: Liquid chromatographic determination of fluoroquinolones in egg albumen and egg yolk of laying hens using fluorometric detection. J Agricult Food Chem 2002, 50, 4452-4455.

5. Gajda A., Posyniak A., Zmudzki J., Gbylik M., Bladek T.: Determination of (fluoro)quinolones in eggs by liquid chromatography with fluorescence detection and confirmation by liquid chromatography tandem mass spectrometry. Food Chem 2012, 135, 430-439.

6. Gbylik M., Posyniak A., Gajda A.: Simultaneous determination of fluoroquinolones in feed by liquid chromatography with fluorescence detection. Bull Vet Inst Pulawy 2012, 56, 267-417.

7. Gorla N., Chiostri E., Ugnia L., Wayers A., Giacomelli N., Davicino R., Ovando G.: HPLC residues of enrofloxacin and ciprofloxacin in eggs of laying hens. Int J Antimicrob Agents 1997, 8, 253-256.

8. Hassouan M.K., Ballesteros O., Taoufiki J., Vilchez J.L., Cabrera-Aguilera M., Navalon A. :Multiresidue determination of quinolone antibacterials in eggs of laying hens by liquid chromatography with fluorescence detection. J Chromatogr B 2007, 852, 625-630.

9. Herranz S., Moreno-Bondi M.C., Marazuela M.D.: Development of a new sample pretreatment procedure based on pressurized liquid extraction for the determination of fluoroquinolone residues in table eggs. J Chromatogr A 2007, 1140, 63-70.

10. Kantiani L., Farré M, Barceló D.: Rapid residue analysis of fluoroquinolones in raw bovine milk by online solid phase extraction followed by liquid chromatography coupled to tandem mass spectrometry. J Chromatogr A 2011, 50, 9019-9027.

11. Martinez M., McDermott P., Walker R.: Pharmacology of the fluoroquinolones: A perpective for the use in domestic animals. Vet J 2006, 172, 10-28.

12. Plackett R.L., Burman J.P.: The design of optimal multifactorial experiments. Biometrika 1946, 33, 305-325.

13. Posyniak A., Mitrowska K.: Analytical procedure for the determination of fluoroquinolones in animals muscle. Bull Vet Inst Pulawy 2008, 52, 427-430.

14. Posyniak A., Zmudzki J., Semeniuk S.: Effects of the matrix and sample preparation on the determination of fluoroquinolone residues in animal tissues. J Chromatogr A 2001, 914, 89-94.

15. Rapid Alert System for Food and Feed (RASFF) Portal:

16. Schneider M., Donoghue D.: Multiresidue determination of fluoroquinolone antibiotics in eggs using liquid chromatography-fluorescence-mass spectrometry. Chim Anal Acta 2003, 483, 39-49.

17. Stahlmann R.: Clinical toxicological aspects of fluoroquinolones. Toxicol Letters 2002, 127, 269-277.

18. Van der HeydenY., Nijhuis A., Smeyers-Verbeke J., Vandeginste B.G.M.: Massart D.L. :Guidance for robustness: ruggedness tests in method validation. J Pharmacol Biomed Anal 2001, 24, 723-753.

19. Walker R.C.: The fluoroquinolones. Mayo Clinic Proc 1999, 74, 1030-1037.

20. Zeng Z., Dong A., Yang G., Chen Z., Huang X.: Simultaneous determination of nine fluoroquinolones in egg white and egg yolk by liquid chromatography with fluorescence detection. J Chromatogr B 2005, 821, 202-209.

Bulletin of the Veterinary Institute in Pulawy

The Journal of National Veterinary Research Institute in Pulawy

Journal Information

IMPACT FACTOR 2017: 0.811
5-year IMPACT FACTOR: 0.973

CiteScore 2017: 0.68

SCImago Journal Rank (SJR) 2017: 0.287
Source Normalized Impact per Paper (SNIP) 2017: 0.484

Cited By


All Time Past Year Past 30 Days
Abstract Views 0 0 0
Full Text Views 118 118 10
PDF Downloads 54 54 3