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Determination of antibiotics such as macrolides, ionophores and tiamulin in liquid manure by HPLC–MS/MS

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Abstract

A method for the analysis of several macrolide and ionophore antibiotics as well as tiamulin in liquid manure was developed. Reversed-phase liquid chromatography and atmospheric pressure chemical ionisation (APCI) tandem mass spectrometry was used for detection.

High-performance liquid chromatographic (HPLC) separation of the antibiotics was achieved in 35 min. The analytes were extracted with ethyl acetate and the extracts were cleaned up by solid-phase extraction on a diol SPE cartridge.

Recovery experiments with spiked liquid manure concentrations varying from 6 to 2,000 µg kg−1 gave constant recovery rates. The recovery rates for the macrolides erythromycin, roxithromycin and oleandomycin were 75–94%, that for the ionophore salinomycin was 119%, while that for the pleuromutilin tiamulin was 123%, when using a macrolide internal standard. The relative standard deviation was found to be 15–36% and the limits of detection were 0.4–11.0 µg kg−1.

The maximum concentrations found in manure samples were 43 µg kg−1 for tiamulin and 11 µg kg−1 for salinomycin.

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Acknowledgements

The authors are indebted to the two farmers in North-Rhine-Westphalia who cooperated in the manure sampling and provided data on the application of antibiotics during conventional farm management. The authors are grateful to Thomas Pfeifer who made a substantial contribution during the method development on the mass spectrometer. This study was supported by the Ministry for Education, Science and Research (MSWF) of North-Rhine-Westphalia (NRW), Germany.

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  1. Institute of Environmental Research, Otto-Hahn-Str. 6, 44227, Dortmund, Germany

    Michael P. Schlüsener, Kai Bester & Michael Spiteller

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  1. Michael P. Schlüsener
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  2. Kai Bester
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  3. Michael Spiteller
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Correspondence to Michael P. Schlüsener.

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Schlüsener, M.P., Bester, K. & Spiteller, M. Determination of antibiotics such as macrolides, ionophores and tiamulin in liquid manure by HPLC–MS/MS. Anal Bioanal Chem 375, 942–947 (2003). https://doi.org/10.1007/s00216-003-1838-9

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  • DOI: https://doi.org/10.1007/s00216-003-1838-9

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