Determination of erythromycin A in salmon tissue by liquid chromatography with ionspray mass spectrometry

From National Research Council Canada

DOIResolve DOI: https://doi.org/10.1002/bms.1200211210
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Name affiliation
  1. National Research Council Canada. NRC Institute for Marine Biosciences
FormatText
TypeArticle
Journal titleBiological Mass Spectrometry
ISSN1052-9306
1096-9888
Volume21
Issue12
Pages675–687
Abstract
A reverse-phase liquid chromatography/mass spectrometry (LC/MS) method, incorporating gradient elution, is described for the characterization of residual erythromycin A and its metabolites in salmon tissue. The method uses ionspray, a mild atmospheric pressure ionization technique which provides an abundant protonated molecule well suited for selected ion monitoring experiments. Tandem mass spectrometry (MS/MS) using collision-induced dissociation was used to provide structural information. The LC/MS method was tested for the analysis of salmon tissue spiked with erythromycin A at levels between 0.01 and 1 p.p.m. A simple extraction and clean-up procedure, slightly modified from that described by Takatsuki et al. (J. Assoc. Off. Anal. Chem. 70, 708 (1987)), was used in this work. Using selected ion and selected reaction monitoring techniques, the LC/MS and LC/MS/MS methods provided detection limits of <10 and 50 ng g−1, respectively. Confirmatory full-scan LC/MS and LC/MS/MS spectra were obtained at the 0.5 and 1 μg g−1 levels, respectively. Using a combination of these techniques, the presence of residual erythromycin A was confirmed in the tissue of fish administered medicated feed containing the antibiotic. In addition, several metabolites and degradation products of erythromycin A, including anhydroerythromycin and N-demethylerythromycin, were detected and where possible confirmed by comparison with authentic compounds. Although this analytical method has been shown to afford the necessary sensitivity and precision, application of these techniques to high-throughput quantitative analyses will require development of an improved clean-up procedure and preferably also of a suitable surrogate internal standard.
Publication date
LanguageEnglish
Peer reviewedYes
NRC number34825
NPARC number23000882
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