Determination of Antimicrobial Residues in Honey by Liquid Chromatography Tandem Mass Spectrometry
Antibiotics are generally used worldwide against bacterial diseases in the treatment of food-producing animals. Since the residues of active agents or their metabolites can appear in these foods, the European Union, for instance, has set maximum residue limit concentrations for authorised veterinary drugs in foodstuffs. However, as yet, regulatory limits have not been established for honey and thus far, only recommendations exist. The aim of this study is to present a multiscreening method for residues in honey for the determination of 36 antimicrobial residues associated with several antibiotics of the B1 group (sulfonamides, trimethoprim, aminoglycosides, tetracyclines, quinolones and lincomycin) as well as the antibiotic griseofulvin. During the screening analysis, samples are hydrolysed in an acidified medium, purified on polymeric solid-phase extraction cartridges and subsequently analysed by reversed phase ion pair liquid chromatography tandem mass spectrometry. The liquid chromatographic separation was optimised by computer simulation with DryLab software. The positive identification of target compounds in suspicious samples was confirmed using earlier developed antibiotic class specific methods of which the aminoglycoside method is herein described in detail. The developed approaches were then applied to samples in the national monitoring program after their successful validation. Moreover, the screening and confirmatory methods were applied to proficiency test samples resulting in satisfactory identification and quantification. However, the analysis of real samples revealed that co-eluting target compounds can have considerable influence on the accuracy of this semi-quantitative multiscreening method.
KeywordsAntimicrobial residues Honey Liquid chromatography tandem mass spectrometry Screening Confirmation Proficiency test
We wish to acknowledge the assist of Éva Pálffi, Tímea Kremniczky and Viktória Lipcsei in the sample preparations. Authors would like to thank Szabolcs Fekete for improving the paper.
Compliance with Ethical Standards
Conflict of Interest
The authors declare that they have no conflict of interest.
This article does not contain any studies with human or animal subjects performed by any of the authors.
Consent for Publication
Publication has been approved by all individual participants.
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