Abstract
A multiclass method has been developed to screen and confirm a wide range of anti-microbial residues in muscle and milk, and validated using liquid-chromatography coupled to (low-resolution, LR) tandem mass spectrometry (LC-QqQ). Over sixty antibiotics, belonging to ten distinct families, were included in the method scope. The development process was rapidly concluded as a result of two previously implemented methods. This consisted of identical sample treatments, followed by liquid chromatography, and coupled with high-resolution (HR) mass spectrometry (LC-Q-Orbitrap). The validation study was performed in the range between 10–1500 μg·kg−1 for muscles and 2–333 μg·kg−1 for milk. The main performance characteristics were estimated and, then, compared to those previously obtained with HR technique. The validity of the method transfer was ascertained also through inter-laboratory studies.
Highlights
Antibiotics are widely used in livestock breeding to treat several diseases that appear in all the food producing animal species
In the last ten years, the improvement of LC-QqQ systems allowed the realization of a further step in drug residue analysis, introducing procedures that are able to determine simultaneously more than one drug class [2–4]
The chromatographic conditions were optimized starting from the parameters set for the LC-Q-Orbitrap methods
Summary
Antibiotics are widely used in livestock breeding to treat several diseases that appear in all the food producing animal species. Surveillance should be aimed at controlling compliance with the maximum residue limits (MRLs), fixed in Table 1 of the Annex of Regulation (EC) No 37/2010 [1]. In the early 2000s, the liquid chromatography coupled to tandem mass spectrometry technique (LC-QqQ) became essential in the routine analysis of single class of veterinary drug residues in food. In the last ten years, the improvement of LC-QqQ systems allowed the realization of a further step in drug residue analysis, introducing procedures that are able to determine simultaneously more than one drug class [2–4]. A remarkable effort has been made to progressively replace single-class with multiclass protocols, since this is a cost-effective way to improve the current residue control programs, thereby ensuring the determination of a wide number of compounds, with only few methods.
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