Determination of Fluoroquinolone Residues in Bovine Kidney Using SPE and LC/MS/MS

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Michael S. Young;Kevin M. Jenkins [Waters]
HPLC 2003
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Oasis MAX 150 mg 6 cc Vac Cartridge
ciprofloxacin, enrofloxacin, sarafloxacin, enofloxacin, flumequine, norfloxacin, ofloxacin, lomefloxacin, danofloxacin
Bovine Kidney
Atlantis dC18 5 µm Steel 4.6 mm 150 mm
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In this presentation we will discuss an LC-MS method for the determination of 9 fluoroquinolone (FLQ) residues (ciprofloxacin, enrofloxacin, sarafloxacin, enofloxacin, flumequine, norfloxacin, ofloxacin, lomefloxacin and danofloxacin) in bovine kidney. The drug residues were extracted from a 2 g kidney sample using acidified ethanol. After centrifugation, the sample extracts were passed through a polymeric, mixed-mode cation-exchange solid-phase extraction cartridge (Oasis MCX) for sample clean-up and enrichment. A novel ion-pairing reagent, nonafluoropentanoic acid (NFPA), was utilized for the subsequent chromatographic separation. This reagent is sufficiently volatile for use with atmospheric ionization mass-spectrometry. Thus, nine FLQs were resolved chromatographically using an isocratic mobile phase consisting of 75:22:3 (v/v) 0.2% NFPA:acetonitrile:methanol. The separation was carried out at 30° C using an Atlantis dC18 analytical column (4.6 x 150 mm, 5 ìm particle size). Positive ion atmospheric pressure chemical ionization (APCI) mass spectrometry was used to quantify and confirm the parent ion (M+H)+ and daughter fragments for each analyte. Detection limits were below 10 ng/g.

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