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 chromatography-tandem mass spectrometry.
ABSTRACT 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.
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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.Food Chemistry 12/2012; 135(4):2612-21. · 3.33 Impact Factor
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ABSTRACT: A simple, rapid and sensitive constant wavelength synchronous fluorescence method is developed for the determination of danofloxacin (DAN) in pharmaceutical formulations and its residue in milk based on Al(III) enhanced fluorescence. The synchronous fluorescence intensity of the system is measured at 435 nm using ∆ λ = 80 nm and an excitation wavelength of 280 nm. A good linear relationship between enhanced fluorescence intensity and DAN concentration is obtained in the range of 3-100 ng mL(-1)(r (2) = 0.9991). The limit of detection (LOD, S/N = 3) of the present method is 0.9 ng mL(-1). The proposed method can be successfully applied to the determination of DAN in pharmaceutical formulations and in milk without serious interferences from common excipients, metal ions and other co-existing substances. The method can be used as a rapid screening to judge whether the DAN residues in milk exceed Maximum Residue Limits (MRLs) or not.Journal of Fluorescence 06/2012; 22(5):1407-13. · 1.79 Impact Factor