Comprehensive analysis of B-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.
Original languageEnglish
Pages (from-to)7859-7874
JournalAnalytical and Bioanalytical Chemistry
Volume405
Issue number24
DOIs
Publication statusPublished - 2013

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Lactams
Poultry
Carbapenems
Liquid chromatography
Cephalosporins
Tandem Mass Spectrometry
Liquid Chromatography
Penicillins
Mass spectrometry
Muscle
biapenem
Anti-Bacterial Agents
Muscles
Hydrolysis
Isotope Labeling
Reaction products
Amides
Isotopes
Design of experiments
Labeling

Keywords

  • beta-lactamase
  • quantitative-analysis
  • ceftiofur resistance
  • escherichia-coli
  • european-union
  • bovine muscle
  • kidney tissue
  • enterobacteriaceae
  • salmonella
  • mechanisms

Cite this

@article{4b2c8e43b4c74a98a9acf45d0de87759,
title = "Comprehensive analysis of B-Lactam antibiotics including penicillins, cephalosporins and carbapenems in poultry muscle using liquid chromatography coupled to tandem mass spectrometry",
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.",
keywords = "beta-lactamase, quantitative-analysis, ceftiofur resistance, escherichia-coli, european-union, bovine muscle, kidney tissue, enterobacteriaceae, salmonella, mechanisms",
author = "B.J.A. Berendsen and H.W. Gerritsen and R.S. Wegh and S.L. Lameris and {van Sebille}, R. and A.A.M. Stolker and M.W.F. Nielen",
year = "2013",
doi = "10.1007/s00216-013-6804-6",
language = "English",
volume = "405",
pages = "7859--7874",
journal = "Analytical and Bioanalytical Chemistry",
issn = "1618-2642",
publisher = "Springer Verlag",
number = "24",

}

TY - JOUR

T1 - Comprehensive analysis of B-Lactam antibiotics including penicillins, cephalosporins and carbapenems in poultry muscle using liquid chromatography coupled to tandem mass spectrometry

AU - Berendsen, B.J.A.

AU - Gerritsen, H.W.

AU - Wegh, R.S.

AU - Lameris, S.L.

AU - van Sebille, R.

AU - Stolker, A.A.M.

AU - Nielen, M.W.F.

PY - 2013

Y1 - 2013

N2 - 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.

AB - 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.

KW - beta-lactamase

KW - quantitative-analysis

KW - ceftiofur resistance

KW - escherichia-coli

KW - european-union

KW - bovine muscle

KW - kidney tissue

KW - enterobacteriaceae

KW - salmonella

KW - mechanisms

U2 - 10.1007/s00216-013-6804-6

DO - 10.1007/s00216-013-6804-6

M3 - Article

VL - 405

SP - 7859

EP - 7874

JO - Analytical and Bioanalytical Chemistry

JF - Analytical and Bioanalytical Chemistry

SN - 1618-2642

IS - 24

ER -