Determination of quinolones in chicken tissues by liquid chromatography with ultraviolet absorbance detection
ABSTRACT This paper presents an analytical method for the determination of quinolones in chicken tissues. The procedure involves pre-treatment by solid-phase extraction (SPE) and subsequent liquid chromatography (LC) with UV absorbance detection. Different SPE disposable cartridges and extractants of the tissue samples were tested, and various columns were systematically tested. The mobile phase was composed of acetonitrile and citric buffer at pH 4.5, with an initial composition of acetonitrile-water (12:88, v/v) and using linear gradient elution. Recoveries were 66-91% in the concentration range 30-300 microg kg(-1). The detector response was linear in this range. The limits of detection were 16-30 microg kg(-1). These values were lower than the maximum residue limits established by the European Union.
SourceAvailable from: Nadezhda A. Stoilova[Show abstract] [Hide abstract]
ABSTRACT: The objective of this study was to present simple, rapid and applicable HPLC-method with fluorescence detection for determination of quinolone-residues in chicken muscle. Presence of antibacterial residia gives reise to risk for health, because of chance by disease, allergy or cancer effect. The residues of ciprofloxacine, enrofloxacine, norfloxacine, danfloxacine, difloxacine, sarafloxacine, oxolinic acid, nalidixic acid and flumequine are extracted with acetonitril. The extract was cleaned with an SPE -procedure with HLB cartridges. Elute was analyzed via Zorbax Eclipse XDB liquid chromatography column. It was used gradient program for eluting and time table program because of the different wave lengths of excitation and emission. INTRODUCTION The quinolones are a group of antibiotics which are used in human and veterinary medicine. They have high activity against gram-positive and gram-negative bacteria. Their activity is shown by inhibiting of DNA-guirase in a bacterial cell , thus destroying it. The use of quinolone-antibiotics has resulted in the presence in food with animal origin. The European Union has established maximum residue limits for those types of chemicals in different type of animal tissues and food with animal origin. The aim is to protect the human health against potential harmful residues [2, 3]. That make necessary to develop and validate sensitive and selective multi-residue screening method for identification and quantification of those type antibiotics.
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ABSTRACT: This paper describes the development of a specific ultra performance LC with electrospray ionization tandem mass spectrometric method for simultaneous determination of 13 quinolones in livestock and fishery products. The procedures involve the sample preparation based on solvent extraction without further clean up procedure. The method was validated according to the FDA guidelines. The limit of detection (LOD) and quantification (LOQ) were lower than 0.1 and 0.4 μg/kg, respectively, and these were below the maximum residue limits (MRLs) established by European Union. Recoveries ranged from 87.5 to 104.7% for livestock products and 83.0 to 100.9% for fishery products. Relative standard deviations (RSD) ranged from 0.4 to 6.0% and 0.9 to 5.7%, respectively. The method was successfully applied to the analysis of quinolones residue. This quantitative method has many advantages including simple preparation, rapid determination, and high sensitivity, which could be applied to the determination of quinolones residues in foodstuff.Food science and biotechnology 10/2013; 22(5):1-9. DOI:10.1007/s10068-013-0201-y · 0.66 Impact Factor
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ABSTRACT: 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.Food Analytical Methods 06/2012; 6(3). DOI:10.1007/s12161-012-9488-1 · 1.80 Impact Factor