Qualitative screening of undesirable compounds from feeds to fish by liquid chromatography coupled to mass spectrometry.

摘要: This paper describes the development, validation, and application of a rapid screening method for detection identification undesirable organic compounds in aquaculture products. A generic sample treatment was applied without any purification or preconcentration step. After extraction samples with acetonitrile/water 80:20 (0.1% formic acid), extracts were centrifuged directly injected LC-HRMS system, consisting ultra-high performance liquid chromatography coupled to hybrid quadrupole time-of-flight mass spectrometry (UHPLC-QTOF MS). qualitative validation carried out over 70 representative compounds, including antibiotics, pesticides, mycotoxins, fish feed fillets spiked at 20 100 μg/kg. At highest level, great majority detected (using most abundant ion, typically protonated molecule) unequivocally identified (on basis presence two accurate-mass measured ions). μg/kg many contaminants could already be detected, although using ions not fully reached some them, mainly due complexity this matrix. Subsequent methodology made it possible find several from target list, such as antibiotic ciprofloxacin, insecticide pirimiphos-methyl, mycotoxins fumonisin B2 zearalenone. retrospective analysis full-spectrum acquisition data provided by QTOF MS also made, either reprocessing injecting samples. allowed tentative other undesirables different those included validated list.