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Rapid analysis of aminoglycoside antibiotics in bovine tissues using disposable pipette extraction and ultrahigh performance liquid chromatography - tandem mass spectrometry

Steven J. Lehotay, Katerina Mastovska, Alan R. Lightfield, Alberto Nuñez, Terry Dutko, Chilton Ng, Louis Bluhm
Journal of chromatography 2013 v.1313 pp. 103-112
amikacin, apramycin, cattle, detection limit, gentamicin, kidneys, liver, mass spectrometry, muscle tissues, neomycin, screening, spectinomycin, streptomycin, tobramycin, ultra-performance liquid chromatography, United States
A high-throughput qualitative screening and identification method for 9 aminoglycosides of regulatory interest has been developed, validated, and implemented for bovine kidney, liver, and muscle tissues. The method involves extraction at previously validated conditions, cleanup using disposable pipette extraction, and analysis by a 3 min ultrahigh-performance liquid chromatography – tandem mass spectrometry (UHPLC-MS/MS) method. The drug analytes include neomycin, streptomycin, dihydrosptreptomycin, and spectinomycin, which have residue tolerances in bovine in the US, and kanamicin, gentamicin, apramycin, amikacin, and hygromycin, which do not have US tolerances established in bovine tissues. Tobramycin was used as an internal standard. An additional drug, paromomycin was also validated in the method, but it was dropped during implementation due to conversion of neomycin into paromomycin. Recoveries from spiking experiments at regulatory levels of concern showed that all analytes averaged 70-120% recoveries in all tissues, except hygromycin averaged 61% recovery. Lowest calibrated levels were as low as 0.005 ug/g in matrix extracts, which approximately corresponded to the limit of detection for screening purposes. Drug identifications at levels