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

Schlüsener, Michael P.; Bester, Kai; Spiteller, Michael
April 2003
Analytical & Bioanalytical Chemistry;Apr2003, Vol. 375 Issue 7, p942
Academic Journal
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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