Multiresidue Method for Simultaneous Determination of Ten Quinolone Antibacterial Residues in Multimatrix/Multispecies Animal Tissues by Liquid Chromatography with Fluorescence Detection: Single Laboratory Validation Study

Abstract

Quinolone antibacterials are veterinary drugs authorized for use in food animal production. The analysis of residual amounts of drugs in food from animal origin is important for quality control of products for consumers. For this purpose, Maximum Residue Limits (MRLs) have been set up by a European Union Council Regulation on Veterinary Drug Residues (No. 90/2377/EEC and subsequent), and 8 quinolones received MRLs at concentration levels depending on both the matrix and the animal species of interest. A method was developed for screening and confirming 10 quinolone residues (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, nalidixic acid, norfloxacin, oxolinic acid, sarafloxacin) in a wide variety of matrixes of different animal species. It involves extraction of the residues from the biological tissues/fluids by acidic aqueous solution, centrifugation and filtration prior to injection on a C18 narrow-bore column, and detection through a 3-step-mode fluorescence detector. The method was validated during a 2-week study for a set of 8 species-matrixes (i.e., bovine raw milk, bovine muscle, porcine muscle, porcine kidney, porcine liver, fish flesh and skin, poultry muscle, whole egg). Residues were quantified down to 15 μg/kg with limits of detection and quantitation ranging from 4 to 11 and 13 to 36 μg/kg, respectively, which are sufficient compared to the wide range of MRLs set for these substances (from 30 μg/kg for danofloxacin in milk to 1900 μg/kg for difloxacin in poultry liver). The limit of performance of the method in terms of CCα and CCβ, the critical concentrations stated in the Decision No. 2002/657/EC and the ISO Standard No. 11843, has been calculated for the authorized (MRL) substances but only estimated in the case of the nonauthorized (non-MRL) substances.

Determination and kinetics of enrofloxacin and ciprofloxacin in Tra catfish (Pangasianodon hypophthalmus) and giant freshwater prawn (Macrobrachium rosenbergii) using a liquid chromatography/mass spectrometry method

“…In the literature, some methods have been developed for the determination of quinolones (QN) and FQ residues in multimatrix ⁄ multispecies animal tissues (Johnston et al, 2002;Marchesini et al, 2007;Toussaint et al, 2002;Van Hoof et al, 2005). Current methods for QN and FQ residue analysis are liquid chromatography (LC) coupled with ultraviolet (UV) and fluorescence detection (FLD) (Roybal et al, 2002;Schneider et al, 2007;Verdon et al, 2005) or mass spectrometric (MS) detection, which is more sensitive and selective (Dufresne et al, 2007;Johnston et al, 2002). Several LC-MS or tandem mass spectrometry (LC-MS ⁄ MS) methods have been described for the confirmation and quantification of FQs in seafood and aquaculture products, such as salmon, trout, gilthead sea bream, as well as shrimp (Dufresne et al, 2007;Johnston et al, 2002;Samanidou et al, 2008).…”

Enrofloxacin assay validation and pharmacokinetics following a single oral dose in chickens

“…High-performance liquid chromatography (HPLC) is the most frequently employed technique in the determination of ENRO and CIPRO in biological fluids (Ovando et al, 1999;Yang et al, 2005), tissues (Gigosos et al, 2000;Garcia et al, 2001;Ovando et al, 2004;Verdon et al, 2005) and dosage forms (Samanidou et al, 2005a) with fluorescence, photodiode array and mass spectrometric detectors. Polymeric stationary phases (Yorke & Froc, 2000;Chu et al, 2002) and octadecyl stationary phases (Horie et al, 1994;Strelevitz & Linhares, 1996;Gorla et al, 1997;Ramos et al, 2003) have been used.…”

Laser diode thermal desorption mass spectrometry for the analysis of quinolone antibiotic residues in aquacultured seafood

“…Numerous analytical methods have been published for the determination of quinolone antibiotics in animal tissues and biological fluids using a variety of techniques. Many recent seafood methods have been based on liquid chromatographic separation with fluorescence or mass spectrometric detection. Methods based on capillary electrophoresis and optical biosensor techniques have also been published for seafood analysis.…”