期刊
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
卷 375, 期 7, 页码 942-947出版社
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-003-1838-9
关键词
agriculture; antibiotics; APCI; HPLC-MS/MS; liquid manure
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 mug 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 mug kg(-1). The maximum concentrations found in manure samples were 43 mug kg(-1) for tiamulin and 11 mug kg(-1) for salinomycin.
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