Abstract
A comprehensive method for the quantitative residue analysis of trace levels of 22 ß-lactam antibiotics, including penicillins, cephalosporins, and carbapenems, in poultry muscle by liquid chromatography in combination with tandem mass spectrometric detection is reported. The samples analyzed for ß-lactam residues are hydrolyzed using piperidine in order to improve compound stability and to include the total residue content of the cephalosporin ceftifour. The reaction procedure was optimized using a full experimental design. Following detailed isotope labeling, tandem mass spectrometry studies and exact mass measurements using high-resolution mass spectrometry reaction schemes could be proposed for all ß-lactams studied. The main reaction occurring is the hydrolysis of the ß-lactam ring under formation of the piperidine substituted amide. For some ß-lactams, multiple isobaric hydrolysis reaction products are obtained, in accordance with expectations, but this did not hamper quantitative analysis. The final method was fully validated as a quantitative confirmatory residue analysis method according to Commission Decision 2002/657/EC and showed satisfactory quantitative performance for all compounds with trueness between 80 and 110 % and within-laboratory reproducibility below 22 % at target level, except for biapenem. For biapenem, the method proved to be suitable for qualitative analysis only.
Original language | English |
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Pages (from-to) | 7859-7874 |
Journal | Analytical and Bioanalytical Chemistry |
Volume | 405 |
Issue number | 24 |
DOIs | |
Publication status | Published - 2013 |
Keywords
- beta-lactamase
- quantitative-analysis
- ceftiofur resistance
- escherichia-coli
- european-union
- bovine muscle
- kidney tissue
- enterobacteriaceae
- salmonella
- mechanisms