An HPLC-DAD method for the simultaneous determination of nine β-lactam antibiotics in ewe milk

•A method for simultaneous determination of nine β-lactams in ewe milk using HPLC-DAD is described.•Sample treatment allowed extracts ready for fast identification and quantification.•Analyte recoveries ranged from 79% to 96% with relative standard deviations between 0.5% and 4.9%.•LOQs were 3.4–8.6...

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Bibliographic Details
Published in:Food chemistry 2013-11, Vol.141 (2), p.829-834
Main Authors: Camara, M, Gallego-Pico, A, Garcinuno, R M, Fernandez-Hernando, P, Durand-Alegria, J S, Sanchez, P J
Format: Article
Language:English
Subjects:
Animals
Anti-Bacterial Agents - analysis
Antibacterial agents
Antibiotic residues
Antibiotics. Antiinfectious agents. Antiparasitic agents
beta-Lactams - analysis
Biological and medical sciences
Chromatography, High Pressure Liquid - instrumentation
Chromatography, High Pressure Liquid - methods
Ewe milk
Food Contamination - analysis
Liquid chromatography
Medical sciences
Milk - chemistry
Pharmacology. Drug treatments
UV-diode array detection
β-lactams
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Summary:•A method for simultaneous determination of nine β-lactams in ewe milk using HPLC-DAD is described.•Sample treatment allowed extracts ready for fast identification and quantification.•Analyte recoveries ranged from 79% to 96% with relative standard deviations between 0.5% and 4.9%.•LOQs were 3.4–8.6μgkg−1, lower than MRLs established by the European Union.•A powerful and popular tool for confirmation of antibiotics in small milk industries is described. The presence of β-lactam residues in foodstuffs constitutes a potential risk to the human health and undesirable effects on consumers, and nowadays these antibiotic residues are also recognised as an emerging environmental problem. In addition, these are of great concern to prestigious Manchego cheese processors (Central Spain denomination of origin) because they reduce the curdling of milk and cause improper cheese ripening, which consequently lead to an important loss of monetary income. This work describes the development of a sensitive and reliable method using liquid chromatography with UV-diode array detection (LC-DAD) for simultaneous determination of the β-lactam antibiotics, ampicillin (AMP), benzylpenicillin (PEG), cephalexin (CFX), cefazolin (CFL), cefoperazone (CFP), cloxacillin (CLO), dicloxacillin (DCL), oxacillin (OXA) and phenoxymethylpenicillin (PEV), in Manchega ewe milk. The column, mobile phase, temperature and flow rate were optimised to provide the best resolution of these analytes. The extraction method of the antibiotic residues involves the deproteinisation of the milk sample using acetonitrile and centrifugation followed by a solid-phase extraction (SPE) clean-up. The recoveries for the studied β-lactams ranged from 79% to 96% with relative standard deviations between 0.5% and 4.9%. The limits of quantification (LOQs) for all these compounds were in the range of 3.4–8.6μgkg−1, which are lower than the maximum residue limits (MRLs) established by the European Union for the studied β-lactams in milk, making the method suitable for performing routine analyses. The proposed multi-residue LC-UV-diode array detection (LC-DAD) method is a powerful and popular alternative for the determination and confirmation of antibiotic residues in small milk industries and is the first one capable of determining nine β-lactam antibiotics in samples of Manchega ewe milk.
ISSN:0308-8146
1873-7072
DOI:10.1016/j.foodchem.2013.02.131