Liquid Chromatography–Tandem Mass Spectrometry Multiclass Method for 46 Antibiotics Residues in Milk and Meat: Development and Validation
- 528 Downloads
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.
- Arsand JB, Jank L, Martins MT et al (2016) Determination of aminoglycoside residues in milk and muscle based on a simple and fast extraction procedure followed by liquid chromatography coupled to tandem mass spectrometry and time of flight mass spectrometry. Talanta 154:38–45. doi: 10.1016/j.talanta.2016.03.045 CrossRefGoogle Scholar
- Bittencourt MS, Martins MT, de Albuquerque FGS et al (2012) High-throughput multiclass screening method for antibiotic residue analysis in meat using liquid chromatography-tandem mass spectrometry: a novel minimum sample preparation procedure. Food Addit Contam Part A 29:508–516. doi: 10.1080/19440049.2011.606228 CrossRefGoogle Scholar
- Bousova K, Senyuva H, Mittendorf K (2013) Quantitative multi-residue method for determination antibiotics in chicken meat using turbulent flow chromatography coupled to liquid chromatography-tandem mass spectrometry. J Chromatogr A 1274:19–27. doi: 10.1016/j.chroma.2012.11.067 CrossRefGoogle Scholar
- Brasil Ministério da Agricultura Pecuária e Abastecimento (2011). Manual de garantia da qualidade analíticaGoogle Scholar
- Coscollà C, León N, Pastor A, Yusà V (2014) Combined target and post-run target strategy for a comprehensive analysis of pesticides in ambient air using liquid chromatography-Orbitrap high resolution mass spectrometry. J Chromatogr A 1368:132–142. doi: 10.1016/j.chroma.2014.09.067 CrossRefGoogle Scholar
- Croubels S, Daeseleire E (2012) Veterinary drug residues in foods. In: Chemical Contaminants and Residues in Food. pp 148–182Google Scholar
- European Commission (2010) Commission regulation (EU) No. 37/2010 of 22 December 2009: on pharmacologically active substances and their classification regarding maximum residue limits in foodstuffs of animal origin. Off. J. Eur. Union 1–72Google Scholar
- European Commission (2002) Decision (2002/657/EC) of 12 August 2002 implementing council directive 96/23/EC concerning the performance of analytical methods and interpretation of results. Off. J. Eur. Communities 8–36Google Scholar
- Hoff RB, Barreto F, Kist TBL (2009) Use of capillary electrophoresis with laser-induced fluorescence detection to screen and liquid chromatography-tandem mass spectrometry to confirm sulfonamide residues: validation according to European Union 2002/657/EC. J Chromatogr A 1216:8254–8261. doi: 10.1016/j.chroma.2009.07.074 CrossRefGoogle Scholar
- Hoff RB, Barreto F, Melo J, et al. (2013) Scope extension validation protocol: inclusion of analytes and matrices in an LC-MS/MS sulfonamide residues method. Food Addit Contam Part A 131106185253008. doi: 10.1080/19440049.2013.861082
- Jank L, Martins MT, Arsand JB et al (2015a) High-throughput method for macrolides and lincosamides antibiotics residues analysis in milk and muscle using a simple liquid-liquid extraction technique and liquid chromatography-electrospray-tandem mass spectrometry analysis (LC-MS/MS). Talanta 144:686–695. doi: 10.1016/j.talanta.2015.06.078 CrossRefGoogle Scholar
- Li N, Feng F, Yang B, et al. (2014) Simultaneous determination of β-lactam antibiotics and β-lactamase inhibitors in bovine milk by ultra performance liquid chromatography-tandem mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci 945–946:110–114. doi: 10.1016/j.jchromb.2013.11.044
- Martins MT, Barreto F, Hoff RB et al (2016) Multiclass and multi-residue determination of antibiotics in bovine milk by liquid chromatography-tandem mass spectrometry: combining efficiency of milk control and simplicity of routine analysis. Int Dairy J 59:44–51. doi: 10.1016/j.idairyj.2016.02.048 CrossRefGoogle Scholar
- Prestes OD, Martins ML, Do A, Friggi C et al (2013) The state of the art in determination of veterinary drug residues in foods of animal origin using chromatographic techniques coupled to mass spectrometry. Quim Nov. 36:697–710. doi: 10.1590/S0100-40422013000500015
- Woodward K (2004) The evolution of safety assessments for veterinary medicinal products the European Union. Vet Hum Toxicol 46:199–205Google Scholar