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

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.

[1]  C. Salisbury,et al.  Determination of tylosin and tilmicosin residues in animal tissues by reversed-phase liquid chromatography. , 1994, Journal of AOAC International.

[2]  M H Montforts,et al.  The exposure assessment for veterinary medicinal products. , 1999, The Science of the total environment.

[3]  B. Jang,et al.  Determination of roxithromycin residues in the flounder muscle with electrospray liquid chromatography-mass spectrometry. , 2000, Journal of chromatography. B, Biomedical sciences and applications.

[4]  G. Bordin,et al.  How to overcome matrix effects in the determination of pesticides in fruit by HPLC–ESI–MS–MS , 2001, Fresenius' journal of analytical chemistry.

[5]  H. Neu,et al.  The Crisis in Antibiotic Resistance , 1992, Science.

[6]  C. A. Russell,et al.  The characterisation of polyether ionophore veterinary drugs by HPLC-electrospray MS. , 1998, The Analyst.

[7]  H. Nau,et al.  Determination of persistent tetracycline residues in soil fertilized with liquid manure by high-performance liquid chromatography with electrospray ionization tandem mass spectrometry. , 2002, Analytical chemistry.

[8]  V. Hormazábal,et al.  DETERMINATION OF AMPROLIUM, ETHOPABATE, LASALOCID, MONENSIN, NARASIN, AND SALINOMYCIN IN CHICKEN TISSUES, PLASMA, AND EGG USING LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY , 2000 .

[9]  S. Furlanetto,et al.  High-performance liquid chromatographic assay of erythromycin from biological matrix using electrochemical or ultraviolet detection. , 2000, The Analyst.

[10]  M. Spiteller,et al.  Binding of Fluoroquinolone Carboxylic Acid Derivatives to Clay Minerals , 1997 .

[11]  T. Ternes,et al.  Determination of antibiotics in different water compartments via liquid chromatography-electrospray tandem mass spectrometry. , 1998, Journal of chromatography. A.

[12]  M. Birkved,et al.  Environmental risk assessment of human pharmaceuticals in Denmark after normal therapeutic use. , 2000, Chemosphere.

[13]  H. Nau,et al.  [Substances with pharmacological effects including hormonally active substances in the environment: identification of tetracyclines in soil fertilized with animal slurry]. , 2000, DTW. Deutsche tierarztliche Wochenschrift.

[14]  M. Spiteller,et al.  Determination of selected sulfonamide antibiotics and trimethoprim in manure by electrospray and atmospheric pressure chemical ionization tandem mass spectrometry. , 2002, Rapid communications in mass spectrometry : RCM.

[15]  B. Halling‐Sørensen,et al.  Acute and chronic toxicity of veterinary antibiotics to Daphnia magna. , 2000, Chemosphere.

[16]  J. Sherma,et al.  Method. II. Liquid chromatographic determination of tiamulin hydrogen fumarate in tiamulin-poly(vinyl chloride) formulations. , 1993, Journal of AOAC International.

[17]  P. Delahaut,et al.  Identification and quantification of five macrolide antibiotics in several tissues, eggs and milk by liquid chromatography-electrospray tandem mass spectrometry. , 2001, Journal of chromatography. B, Biomedical sciences and applications.

[18]  R. Angeletti,et al.  Determination of tylosin residues in pig tissues using high-performance liquid chromatography. , 1998, The Analyst.

[19]  J. Chantot,et al.  New ether oxime derivatives of erythromycin A. A structure-activity relationship study. , 1991, The Journal of antibiotics.

[20]  A. Hogenboom,et al.  Analytical strategies for the screening of veterinary drugs and their residues in edible products. , 1995, Journal of chromatography. B, Biomedical applications.

[21]  S. Jørgensen,et al.  Drugs in the environment. , 2000, Chemosphere.