Simultaneous Determinaton of Fluoroquinolones in Feed by Liquid Chromatography with Fluorescence Detection

Małgorzata Gbylik 1 , Andrzej Posyniak 1  and Anna Gajda 1
  • 1 Department of Pharmacology and Toxicology, National Veterinary Research Institute, 24-100 Pulawy, Poland


An HPLC method with fluorescence detection (HPLC-FLD) was developed for the simultaneous quantitative determination of enrofloxacin, ciprofloksacin, sarafloxacin, and difloxacin in feed. The samples were extracted with 0.25% formic acid in ultrasonic bath and purified by solid phase extraction (SPE) on Strata-X cartridges. The samples were analysed on Luna C8 liquid chromatography column with gradient programme by acetonitrile and 0.025 M phosphoric acid with 0.0025 M sodium 1- heptanesulfonate monohydrate. The method was successfully validated according to the requirements of the European Decision 2002/657/EC. Recoveries of the components from spiked feed samples ranged from 55%-70%. Repeatability was <7%. The method presented here proved to be efficient, rapid, and a selective approach for determination of fluoroquinolones in feed.

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  • 1. Ballesteros O., Toro I., Sanz-Nebot V., Navalón A., Vilchez J., Barbosa J.,: Determination of fluoroquinolones in human urine by liquid chromatography coupled to pneumatically assisted electrospray ionization mass spectrometry. J Chromatogr B 2003, 1, 137-144.

  • 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. Off Publ Europ Comm 2002, L 221, 8-36.

  • 3. 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,

  • 4. Hanwen S., Lixin W., Xiaolan O., Xusheng G.: Simultaneous determination of malachite green, enrofloxacin and ciprofloxacin in fish farming water and feed by liquid chromatography with solid-phase extraction. Environmental Monitoring Assessment 2011, 179, 421-429.

  • 5. Haoyan X., Tianyi W., Qi Z., Hui W., Yang X., Xiaopan Z., Feng W., Lan D.: Analysis of fluoroquinolones in animal feed based on microwave-assisted extraction by LC-MS-MS determination. Chromatographia 2011, 74, 267-274.

  • 6. Jimenez-Lozano E., Marques I., Barron D., Beltran J.L., Barbosa J.: Determination of pKa values of quinolones from mobility and spectroscopy data obtained by capillary electrophoresis and diode array detector. Anal Chim Acta 2002, 464, 37-45.

  • 7. 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.

  • 8. Pecorelli I., Galarini R., Bibi R., Floridi A., Casciarri E., Floridi A.: Simultaneous determination of 13 quinolones from feeds using accelerated solvent extraction and liquid chromatography. Anal Chim Acta 2003, 483, 81-89.

  • 9. Posyniak A., Mitrowska K.: Analytical procedure for the determination of fluoroquinolones in animal muscles. Bull Vet Inst Pulawy 2008, 52, 427-430.

  • 10. 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.

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

  • 12. Wolfson J.S., Hooper D.C.: The fluoroquinolones: structure, mechanisms of action and resistance, and spectra activity in vitro. Am Soc Microbiol 1985, 28, 581-586.


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