Development and validation of an HPLC confirmatory method for residue analysis of ten quinolones in tissues of various food‐producing animals, according to the European Union Decision 2002/657/EC

Abstract

The aim of this work was to develop an HPLC method for the simultaneous determination of ten quinolones: enoxacin, ofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, oxolinic acid, nalidixic acid, and flumequine, in various tissues of food-producing animals. Separation was achieved on a PerfectSil Target column (250 mm x 4 mm, ODS-3, 5 microm), by MZ-Analysentechnik (Germany), at room temperature. The mobile phase consisted of 0.1% TFA-CH(3)OH-CH(3)CN and was delivered by a gradient program of 35 min. The detection and quantitation was performed on a photodiode array detector at 275 and 255 nm. Caffeine (7.5 ng/microL) was used as the internal standard (IS). Analytes were isolated from tissue samples by 0.1% methanolic TFA solution. SPE, using LiChrolut RP-18 cartridges, was applied for further purification. The extraction protocol was optimized and the final recoveries varied between 92.0 and 107.4%. The method was fully validated according to Commission Decision 2002/657/EC. Limits of quantitation for the examined quinolones extracted from each tissue were much lower than the respective Maximum Residue Levels, ranging between 30 and 50 microg/kg for bovine tissue, between 30 and 55 microg/kg for ovine tissue, and between 40 and 50 microg/kg for porcine tissue.

Determination of enoxacin and ofloxacin by capillary electrophoresis with electrochemiluminescence detection in biofluids and drugs and its application to pharmacokinetics

“…Therefore, it has become more and more important to develop sensitive and rapid method for the determination of the content of FQs antibiotics in biochemical analysis. Recently, HPLC/LC (Christodoulou et al, 2007;Xiao et al, 2008;EspinosaMansilla et al, 2005;Cañada-Cañada et al, 2007), fl ow injection analysis (Chen et al, 2008;Zhang et al, 2005;Rao et al, 2000) and CE (Lü et al, 2005;Horstkötter and Blaschke, 2001;McCourt et al, 2003;Liu et al, 2008b;Lin et al, 2004;Fan et al, 2007;Yin et al, 2004) have been used in the determination of enoxacin and/or ofl oxacin. In CE methods, the detection modes used mainly included UV-vis (Lü et al, 2005), laser-induced fl uorescence (Horstkötter et al, 2001), mass spectrometry (McCourt et al, 2003), CL (Liu et al, 2008b), photodiode array detection (Lin et al, 2004) and potential gradient detection (Fan et al, 2007).…”

“…They inhibit bacterial DNA-gyrase in cells so that the bacteria cannot reproduce and eventually die (Yoke and Froc, 2000). These compounds have demonstrated activities against Grampositive and Gram-negative bacteria, so they have been broadly applied in the clinical treatment of certain infections, such as prostate, skin, pulmonary, digestive and urinary tract infections, because of good absorption and low frequency of adverse eff ect (Christodoulou et al, 2007). In addition, they are also used for prophylaxis and as feed additives for mass gain promotion (Mitani and Kataoka, 2006).…”

Single‐step extraction followed by LC for determination of (fluoro)quinolone drug residues in muscle, eggs, and milk

“…The stock solutions were stored at 41C for no longer than a couple of months, with the exception of FLUME, NALI, and OXO, which were stable only for a couple of weeks [6]. The working solutions for HPLC injections were prepared daily from the stock solution in a solvent mixture of acetonitrile and 0.01 M oxalic acid (17:83, v/v).…”

“…In order to mitigate these hazards, the European Union has regulated the use of quinolones in food-producing animals [5]. Additionally, the European Union has established the specific Decision 2002/657/EC, which concerns procedures for the validation of analytical methods, to ensure the quality and comparability of analytical results and the interpretation of results in the official control of residues in foodproducing animals [6]. Overall, the analysis of residual quantities of drugs in foods of animal origin is crucial for the quality control of consumer products.…”

Development of an HPLC multi‐residue method for the determination of ten quinolones in bovine liver and porcine kidney according to the European Union Decision 2002/657/EC

“…The extraction step was followed by a further clean-up step by SPE. The solid phase extraction protocol was based on previous studies [20]. The sample was added to LiChrolut RP-18 SPE cartridges which had been previously conditioned with methanol and water.…”