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Updated: May 29, 2026

Quantification of Metal Leaching in Immobilized Metal Affinity Chromatography
Published on: January 17, 2020
Determination of residual fluoroquinolones in honey by liquid chromatography using metal chelate affinity
Yoh-Ichi Yatsukawa1, Hironobu Ito, Takahiro Matsuda
1Japan Food Research Laboratories, 7-4-41, Saitoasagi, Ibaraki, Osaka, 567-0085, Japan. yatsukaway@jfrl.or.jp
Abstract:
A new analytical method for the simultaneous determination of seven fluoroquinolones, namely, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin, especially in dark-colored honey, has been developed. Fluoroquinolone antibiotics were extracted from samples with MacIlvaine buffer solution (pH 4.0) containing EDTA disodium salt dihydrate. The extracts were treated with both a polymeric cartridge and a metal chelate affinity column preloaded with ferric ion (Fe3+). LC separation with fluorescence detection was performed at 40 degrees C using an Inertsil ODS-4 analytical column (150 x 4.6 mm, 3 microm). The mobile phase was composed of 20 mM/L citrate buffer solution (pH 3.1)-acetonitrile mixture (70 + 30, v/v) containing 1 mM/L sodium dodecyl sulfate. Lomefloxacin was used as an internal standard. The developed method was validated according to the criteria of European Commission Decision 2002/657/EC. Decision limits and detection capabilities were below 2.9 and 4.4 microg/kg, respectively.
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