1. Single-laboratory validation of an LC-MS/MS method for determining florfenicol (FF) and florfenicol amine (FFA) residues in chicken feathers and application to a residue-depletion study
- Author
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Ricardo Riquelme, Aldo Maddaleno, Cristóbal Briceño, Javiera Cornejo, C Araya‐Jordan, B. San Martín, and Ekaterina Pokrant
- Subjects
Florfenicol ,Analyte ,Health, Toxicology and Mutagenesis ,Metabolite ,Guidelines as Topic ,010501 environmental sciences ,Toxicology ,01 natural sciences ,Acetone ,chemistry.chemical_compound ,Limit of Detection ,Tandem Mass Spectrometry ,Animals ,0105 earth and related environmental sciences ,Thiamphenicol ,Detection limit ,Methylene Chloride ,Residue (complex analysis) ,Chromatography ,010401 analytical chemistry ,Extraction (chemistry) ,Public Health, Environmental and Occupational Health ,Broiler ,General Chemistry ,General Medicine ,Feathers ,Reference Standards ,Drug Residues ,Anti-Bacterial Agents ,0104 chemical sciences ,Standard curve ,Chloramphenicol ,chemistry ,Solvents ,Chickens ,Chromatography, Liquid ,Food Science - Abstract
A suitable analytical method is required to study the behaviour of florfenicol (FF) and its metabolite florfenicol amine (FFA) in broiler’s feathers. An LC-MS/MS method was developed, assessed and intra-laboratory-validated for FF and FFA analyses. We chose cloramphenicol-d5 as an internal standard, acetone as a solvent for the extraction of the analytes and dichloromethane for the clean-up. Through LC-MS/MS analysis, we established a detection limit of 20 μg kg–1, as well as calculated quantification limits of 24.4 and 24.5 μg kg–1 for FF and FFA, respectively. Validation parameters such as linearity, recovery and precision were calculated following Commission Decision 2002/657/EC. For linearity, all standard curves showed a standard coefficient greater than 0.99. Recoveries ranged from 99% to 102% for all studied concentrations. The results show that this analytical method is precise and reliable. For the depletion study, 64 Ross 308 broilers were treated with a therapeutic dosage of 10% FF duri...
- Published
- 2016