Simultaneous Determination of Nine Quinolones in Food by Liquid Chromatography with Fluorescence Detection

• Published in: Food analytical methods 2013-06, Vol.6 (3), p.803-813
• Main Authors: Stoilova, Nadezhda A., Surleva, Andriana R., Stoev, Georgi
• Format: Article
• Language: English
• Subjects: Analytical Chemistry; Chemistry; Chemistry and Materials Science; Chemistry/Food Science; Food Science; Microbiology
• ISSN: 1936-9751; 1936-976X
• DOI: 10.1007/s12161-012-9488-1

A confirmatory analytical method for simultaneous determination of nine regulated quinolones (Council Regulation 2377/90/ECC) in six matrices of animal origin is proposed. The sample pretreatment involves double step liquid extraction with acetonitrile and purification by solid-phase extraction on Oasis HLB cartridges. The quinolones were separated by liquid chromatography on C18 Zorbax column with gradient elution program. Aqueous formic acid, methanol, and acetonitrile were used as a mobile phase. A multi-wavelength excitation/emission program was used for sensitive fluorescence detection of quinolones. The proposed sample pretreatment protocol was applied to each of the six studied matrices without any modification. The method was validated according to Commission Decision 2002 /657 EC. Residues were quantified down to 15 μg kg −1 with limits of detection and quantification ranging from 3 to 50 μg kg −1 and from 7.5 to 100 μg kg −1 , respectively. The recoveries at the maximum residual limits (MRLs) were between 77 and 120 % with RSD values lower than 30 %. For quinolones without established MRL or maximum required performance limit, the accuracy and precision of the method were estimated at concentration levels corresponding to the lowest linear calibration point and recoveries between 70 and 130 % were achieved. Decision limits, detection capability, and linear range in eggs, milk, fish, ovine muscle, chicken muscle, and porcine kidney are also reported.