作者: Steven J. Lehotay , Katerina Mastovska , Alan R. Lightfield , Alberto Nuñez , Terry Dutko
DOI: 10.1016/J.CHROMA.2013.08.103
关键词:
摘要: A high-throughput qualitative screening and identification method for 9 aminoglycosides of regulatory interest has been developed, validated, implemented bovine kidney, liver, muscle tissues. The involves extraction at previously validated conditions, cleanup using disposable pipette extraction, analysis by a 3 min ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method. drug analytes include neomycin, streptomycin, dihydrosptreptomycin, spectinomycin, which have residue tolerances in the US, kanamicin, gentamicin, apramycin, amikacin, hygromycin, do not US established Tobramycin was used as an internal standard. An additional drug, paromomycin also method, but it dropped during implementation due to conversion neomycin into paromomycin. Proposed fragmentation patterns monitored ions each analyte were elucidated with aid high resolution MS quadrupole-time-of-flight instrument. Recoveries from spiking experiments levels concern showed that all averaged 70-120% recoveries tissues, except hygromycin 61% recovery. Lowest calibrated low 0.005 μg/g matrix extracts, approximately corresponded limit detection purposes. Drug identifications <0.05 made spiked and/or real samples tissues tested. Analyses 60 20 slaughtered cattle screened positive this worked well practice. UHPLC-MS/MS several advantages compared previous microbial inhibition assay, especially distinguishing individual drugs mixture improving gentamicin tissue samples.