High precision and selectivity for quantitation of enrofloxacin and ciprofloxacin in five chicken tissues using solid phase extraction and ESI LC-MS/MS for application in monitoring residues

Abstract

Fluoroquinolones (FQs) are synthetic antimicrobials commonly used in intensive poultry farming to treat chronic respiratory disease, colibacillosis, and fowl cholera. As these drugs are also important in treating infections in humans, their use in poultry has been restricted in some countries to avoid the development of antimicrobial-resistant bacteria. In this work, a novel simple and efficient LC-MS/MS method using solid phase extraction (SPE), ESI ionization and multiple reaction mode (MRM) has been developed and validated to determine the two most common FQ residues: enrofloxacin (ENR) and ciprofloxacin (CIP) in chicken target tissues (muscle, liver, kidney, fat and skin) and in plasma. The method is shown to be sensitive, with limits of quantification (LOQ) between 1 ng g À1 and 5 ng g À1 , recoveries 93-115% and correlation coefficients greater than 0.99. This novel methodology allows faster and simpler sample workflow compared to previously reported methodologies, making it ideal for high-throughput screening and confirmation of both ENR and CIP meeting the international regulation levels.

Tissue depletion study of enrofloxacin and its metabolite ciprofloxacin in broiler chickens after oral administration of a new veterinary pharmaceutical formulation containing enrofloxacin

“…ENR and CIP concentrations in target tissues were determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS) using electrospray as ionization source (ESIþ) (Ferrari et al, 2015). The developed analytical method was validated taking into consideration the European Decision Commission 2002/657/EC (EC, 2002) and the International Cooperation on Harmonization of Technical Requirements for Registration of Veterinary Medicinal Products requirements (VICH, 1999).…”

“…Traditionally, fluoroquinolone (FQ) residue determination levels have been based on analytic methods such as liquid chromatography (LC) with ultraviolet detector (Bailac et al, 2004;Yu et al, 2012), diode array (DAD) (Moema et al, 2012), fluorescence (Garcia-Ovando et al, 2000;Garcia et al, 2001;Pena et al, 2010;Severo, 1999), mass spectrometry (Bailac et al, 2006;Bousova et al, 2013;Ferrari et al, 2015;San Martín et al, 2007;San Martín et al, 2009;Yu et al, 2012) or capillary electrophoresis (Barr on et al, 2001). Currently, the major challenge for main research centers is to keep methodologies updated in order to meet commercial and tread requirements and ensure human health integrity.…”

“…This study refers to a new veterinary pharmaceutical formulation (contains a nominal concentration of 25% ENR) and describes the rate of depletion of ENR and its metabolite CIP in edible tissues of healthy broiler chickens after multiple-dose oral administration (by gavage) using liquid chromatography-tandem mass spectrometry (LC-MS/MS), a sensitive methodology with excellent quality parameters and reduced time of analysis (Barbosa et al, 2009;Ferrari et al, 2015) to determine its withdrawal period.…”

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“…At the same time for the quantification of the analyte from marketed formulations and in bulk a proper sample preparation procedure is often required when the excepients in formulations (suspensions, lotions, creams) interferes with the analyte 36 . In such cases sample pretreatment is often necessary [27][28][29][30][31][32][33][34][35][36] . Thus possible chromatographic interferences and clogging or detoriation of the column can be avoided.…”

“…A number of chromatographic techniques have been developed in last two decades for the quantification of newer fluoroquinolones 14-22 from a variety of sample matrices. The introduction of chromatographic techniques has revolutionized the process of detection, separation and quantification of the parent components and the respective metabolites with higher selectivity, sensitivity, precession and accuracy form a variety of sample matrices including biological and environmental matrices [22][23][24][25][26][27][28][29][30][31][32][33][34][35] . Moreover these chromatographic techniques can be derived from available techniques with slight modification or can be developed on the basis of knowledge gathered through experience and physical properties of the analyte under consideration.…”