Liquid Chromatography–Tandem Mass Spectrometry Multiclass Method for 46 Antibiotics Residues in Milk and Meat: Development and Validation
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A screening method for analysis of 46 antibiotics residues, belonging to different classes, such as tetracyclines, sulfonamides, fluoroquinolones, β-lactams, cephalosporins, macrolides and other minority groups was developed and validated for application in bovine milk and bovine, swine, poultry, equine, fish and shrimp meat samples. Sample preparation consists in solvent extraction followed by clean up with C18 bulk and low temperature purification. Instrumental analysis was performed using liquid chromatography coupled to tandem mass spectrometry system. Chromatographic separation was achieved using a C18 column. Mobile phase was composed by methanol and water. The method was validated according to Commission Decision 2002/657/EC criteria. Validation parameters such as specificity and detection capability (CCβ) were determined and considered suitable to the established criteria. Values of CCβ ranged from 1.0 to 50.0 μg L−1 or μg Kg−1, depending on the compound and the matrix. The proposed method has been applied into Brazilian National Residue Control Plan since 2013 for the determination of antibiotic residues. A total of 3833 samples were analyzed until the current date and 13 samples showed positive results with concentrations above the permitted. The method is fast, easy and adequate for high throughput analysis in routine laboratories.
KeywordsAntibiotics Residues Milk Muscle LC-MS/MS Time of flight mass spectrometry
The authors would like to thank the CAPES for the fellowships provided for Juliana Bazzan Arsand, and to National Council for Scientific and Technological Development (CNPq) for the fellowship provided to Magda Targa Martins, Tanara Magalhães Campos Motta and Tiago Corrêa Feijó.
Compliance with Ethical Standards
Conflict of Interest
Louise Jank declares that they have no conflict of interest. Juliana Bazzan Arsand that they have no conflict of interest. Tanara Magalhães Campos Motta that they have no conflict of interest. Tiago Corrêa Feijó that they have no conflict of interest. Tamara dos Santos Castilhos that they have no conflict of interest. Rodrigo Barcellos Hoff that they have no conflict of interest. Fabiano Barreto that they have no conflict of interest. Tânia Mara Pizzolato that they have no conflict of interest.
This article does not contain any studies with human participants or animals performed by any of the authors.
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