Development of analytical methods for multiresidue determination of quinolones in pig muscle samples by liquid chromatography with ultraviolet detection, liquid chromatography-mass spectrometry and liquid chromagraphy-tandem mass spectrometry
This paper presents a comparison between liquid chromatography with ultraviolet detection (LC-UV), liquid chromatography-mass spectrometry (LC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods developed for the multiresidue determination of 8 quinolones, around their maximum residue levels (MRLs) in pig muscle. The procedure involves common extraction of the quinolones from the tissues by traditional extraction, a step for clean-up and preconcentration of the analytes by solid-phase extraction (SPE) and a subsequent liquid chromatographic analysis. The methods present satisfactory results of linearity, precision and limits of quantification much lower than the MRLs established by the European Union for quinolones in pig tissues.
"LC–UV can be used to determine antibiotics (Benito-Peña et al., 2006; Samanidou et al., 2007), but such methods sometimes present a lack of sensitivity. These techniques have therefore been replaced by methods that use mass spectrometry to provide more specific determination leading to unequivocal confirmation of the compounds studied (Becker, Zittlau, & Petz, 2004; Gentili et al., 2005; Granelli & Branzell, 2007; Hermo, Barrón, & Barbosa, 2008; Kantiani, Farré, & Barceló, 2009; Kantiani, Farré, Sibum, et al., 2009; Marazuela & Bogialli, 2009; Martínez-Huélamo, Jiménez- Gámez, Hermo, Barrón, & Barbosa, 2009; Yamada, Kozono, Ohmori, Morimatsu, & Kitayama, 2006). Some of these authors report the use of tandem mass spectrometry for the simultaneous identification and quantification of target residues in complex matrices. "
[Show abstract][Hide abstract] ABSTRACT: A multiresidue analysis method was developed to determine the content of penicillins in bovine, porcine and chicken muscle tissues. The procedure involves solid phase extraction (SPE) and subsequent analysis by liquid chromatography coupled with tandem mass spectrometry detection (LC-MS/MS) set by the European Union (EU) for all compounds. The method was validated according to EU guideline 2002/657/EC. The LOQ in tissues are below the maximum residue limits (MRLs) and appropriate quality parameters in terms of linearity, accuracy (recoveries higher than 70% for all antibiotics and animal tissues except for AMOX with 50% of recovery) and precision (in terms of intra and inter day with values lower than 12% in all cases) are obtained for the developed method. A study concerning to the matrix effect was made and it was concluded that similar matrix effect could be found in beef, pig and chicken. The method was applied to the analysis of samples of chicken from animals treated with amoxicillin.
"In previous studies, analyses of quinolones from food samples by LC-UV were performed with 10 mM citric acid with different percentages of MeCN at pH 4.5 using a gradient elution timetable (Garcés et al., 2006; Hermo et al., 2006; Bailac et al., 2004). When the biological sample is cow or pig plasma, the pH of the mobile phase should to be changed to pH 5.0 in order to obtain better resolution between peaks of SAR and DIF. "
[Show abstract][Hide abstract] ABSTRACT: This paper presents the multiresidue determination of the series of quinolones regulated by the European Union (marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid and flumequine) in bovine and porcine plasma using capillary electrophoresis and liquid chromatography with ultraviolet detection (CE-UV, LC-UV), liquid chromatography-mass spectrometry and -tandem mass spectrometry (LC-MS, LC-MS/MS) methods. These procedures involve a sample preparation by solid-phase extraction for clean-up and preconcentration of the analytes before their injection into the separation system. All methods give satisfactory results in terms of linearity, precision, accuracy and limits of quantification. The suitability of the methods to determine quinolones was evaluated by determining the concentration of enrofloxacin and ciprofloxacin in real samples from pig plasma and cow plasma.
"Many studies have been published in the literature on multiresidue analysis of quinolones in biological samples and animal tissues (Carlucci, 1998; Hernández- Arteseros et al., 2002; Samanidou et al., 2005). Most of them involve liquid chromatography with ultraviolet (LC–UV; Gigosos et al., 2000; Pecorelli et al., 2003; Bailac et al., 2004; Christodoulou and Samanidou, 2007), fluorescence (LC–FD; Eng et al., 1998; Hernández- Arteseros et al., 2000; Chu et al., 2002; Espinosa- Mansilla et al., 2005; Hassouan et al., 2007) or mass spectrometric detection (Van Vyncht et al., 2002; Toussaint et al., 2002, 2005a,b; Schneider et al., 2005; Van Hoof et al., 2005; Hermo et al., 2006; Bailac et al., 2006; Rubies et al., 2007). "
[Show abstract][Hide abstract] ABSTRACT: A new liquid chromatography-mass spectrometry (LC-MS) method has been developed and validated for the simultaneous determination of eight quinolone antibacterials for veterinary use in processed bovine milk samples. The quinolones studied included marbofloxacin, ciprofloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid and flumequine. Also, a new sample-treatment procedure was used for extraction and preconcentration of these compounds. It involved defatting by centrifugation, protein precipitation by adding a mixture of glacial acetic acid-acetonitrile and removing acetonitrile with dichloromethane; finally, the acidified aqueous layer was evaporated to dryness in a speed vac system, resuspended in the mobile phase and filtered prior to LC injection. The mobile phase was composed of a formic acid aqueous solution 0.1% (v/v) and acetonitrile, with an initial composition of water-acetonitrile 95: 5 (v/v) and using linear gradient elution. Norfloxacin was used as internal standard. The limits of quantification found (2-7 ng g(-1)) were in all cases lower than the maximum residue limits tolerated by the European Union for these compounds in milk.
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