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Comprehensive analysis of ß-lactam antibiotics including penicillins, cephalosporins, and carbapenems in poultry muscle using liquid chromatography coupled to tandem mass spectrometry

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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.

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Acknowledgments

This project was financially supported by the Dutch Ministry of Economic affairs (project 1217261301). We thank Dr. Ton Marcelis for his assistance in the elucidation of the hydrolysis reactions.

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Authors and Affiliations

  1. RIKILT, Wageningen University and Research Centre, Akkermaalsbos 2, 6708WB, P.O. Box 230, 6700AE, Wageningen, The Netherlands

    Bjorn J. A. Berendsen, Henk W. Gerritsen, Robin S. Wegh, Steven Lameris, Ralph van Sebille, Alida A. M. Stolker & Michel W. F. Nielen

  2. Laboratory of Organic Chemistry, Wageningen University, Dreijenplein 8, 6703HB, Wageningen, The Netherlands

    Michel W. F. Nielen

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  1. Bjorn J. A. Berendsen
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  2. Henk W. Gerritsen
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  5. Ralph van Sebille
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  6. Alida A. M. Stolker
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  7. Michel W. F. Nielen
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Correspondence to Bjorn J. A. Berendsen.

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Published in the topical collection Rapid Detection in Food and Feed with guest editors Rudolf Krska and Michel Nielen.

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Berendsen, B.J.A., Gerritsen, H.W., Wegh, R.S. et al. Comprehensive analysis of ß-lactam antibiotics including penicillins, cephalosporins, and carbapenems in poultry muscle using liquid chromatography coupled to tandem mass spectrometry. Anal Bioanal Chem 405, 7859–7874 (2013). https://doi.org/10.1007/s00216-013-6804-6

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