title: Determination of selected sulfonamide antibiotics and trimethoprim in manure by electrospray and atmospheric pressure chemical ionization tandem mass spectrometry.
abstract: A method for the determination of sulfonamides and trimethoprim in the complex matrix liquid manure has been developed using reversed-phase liquid chromatography and atmospheric pressure chemical ionization (APCI) tandem mass spectrometry. A comparison was made between electrospray and atmospheric pressure chemical ionization. APCI proved to be more robust and less sensitive to matrix effects. High-performance liquid chromatographic (HPLC) separation of the analytes was achieved in less than 7 min. The compounds were extracted with ethyl acetate and the extracts were cleaned up by solid-phase extraction on an aminopropyl column. Recoveries were not dependent on the concentration level. The mean recoveries were as follows: trimethoprim 79.0%, sulfadiazine 80.5%, N(4)-acetylsulfadiazine 91.0%, sulfamerazine 78.6%, sulfadimidine 77.2% and sulfamethoxazole 82.8%. Linearity was established over a concentration range of 5 to 5000 microg/kg with correlation coefficients greater than 0.99. The method had a limit of quantitation (LOQ) of 5 microg/kg manure.
authors.affiliation: AWD/elbion, Meissner Str. 191, D-01445 Radebeul, Germany. Thomas.Pfeifer@elbion.de
authors.forename: Thomas
authors.initials: T
authors.lastname: Pfeifer
authors.forename: Jochen
authors.initials: J
authors.lastname: Tuerk
authors.forename: Kai
authors.initials: K
authors.lastname: Bester
authors.forename: Michael
authors.initials: M
authors.lastname: Spiteller
mesh_terms: D000818:Animals; D000890:Anti-Infective Agents / Q000737:chemistry*; D000892:Anti-Infective Agents, Urinary / Q000032:analysis*; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D007202:Indicators and Reagents; D008372:Manure / Q000032:analysis*; D015203:Reproducibility of Results; D012989:Soil Pollutants / Q000032:analysis*; D012997:Solvents; D021241:Spectrometry, Mass, Electrospray Ionization; D013449:Sulfonamides / Q000737:chemistry*; D013552:Swine; D014295:Trimethoprim / Q000032:analysis*
chemical_list: D000890:Anti-Infective Agents; D000892:Anti-Infective Agents, Urinary; D007202:Indicators and Reagents; D008372:Manure; D012989:Soil Pollutants; D012997:Solvents; D013449:Sulfonamides; D014295:Trimethoprim