Validation of a procedure to quantify oxolinic acid, danofloxacin, ciprofloxacin and enrofloxacin in selected meats by micellar liquid chromatography according to EU Commission Decision 2002/657/EC

Abstract

The suitability of an analytical method to determine oxolinic acid, danofloxacin, ciprofloxacin and enrofloxacin in edible tissues, based on micellar liquid chromatogra- phy coupled with fluorescence detection, to be applied in chicken, turkey, duck, lamb, goat, rabbit and horse muscle, is described. The method was fully matrix-matched in-lab revalidated, for each antimicrobial drug and meat, following the guidelines of the EU Commission Decision 2002/657/EC. The permitted limits were the maximum residue limits stated by the EU Commission Regulation 37/2010. The results obtained for the studied validation parameters were in agreement with the guidelines: selectivity (the an- tibiotics were resolved), linearity (r 2 ⬎ 0.995), limit of detection (0.004–0.02 mg/kg), limits of quantification (0.01–0.05 mg/kg), calibration range (up to 0.5 mg/kg), recovery (89.5– 105.0%), precision (⬍8.3%), decision limit, detection capability, ruggedness, stability and application to incurred samples. The method was found to be able to provide reliable con- centrations with low uncertainty within a large interval, including the maximum residue limits, and then was useful to find out prohibited contaminated samples. The method did not require to be adapted for these matrices, and then it maintained its interesting advan- tages: short-time, eco-friendly, safe, inexpensive, easy-to-conduct, minimal manipulation and useful for routine analysis.