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KMID : 1023520070300010013
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Korean Journal of Veterinary Service
2007 Volume.30 No. 1 p.13 ~ p.21
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Study on analytical method of fluoroquinolone residues in eggs by LC/MS/MS
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Choi Yu-Jeong
Yun I-Ran
Nam Sang-Yun
Park Young-Ho
Kim Byeong-Hun
Son Seong-Gi
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Abstract
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An atmospheric pressure chemical ionization (APcI) LC/MS/MS method was developed for the simultaneous analysis of fluoroquinolones (norfloxacin, ciprofloxacin, enrofloxacin, danofloxacin) residues in eggs. The spiked and blank samples were extracted from whole eggs using 50mM phosphate buffer (pH 7.4). The extract was cleaned up by passage though MAX extraction cartridge for solid-phase extraction followed by elution with 4% formic acid in methanol. The extract of sample was separated on a Waters reversed-phase column () and analyzed by APcI positive mode mass spectrometry. The mobile phase consists of aqueous 0.2% nonafluoropentanoic acid (NFPA) and methanol. Multiple reaction monitoring (MRM) using the precursor to product ion combinations of m/z and m/z were used to quantify norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR) and danofloxacin (DAN), respectively. The limits of quantification (LOQ) were 7.8ppb for NOR, 8.5ppb for CIP, 8.9ppb for ENR, and 4.8ppb for DAN. Average recoveries of fortified sample at levels of 0.025 to 0.1 ppm were estimated 71.29% for NOR, 75.27% for CIP, 85.51% for ENR and 81.22% for DAN. These results could be applied for the confirmation and quantification in eggs.
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KEYWORD
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Fluoroquinolones, Eggs, LC/MS/MS, APcI
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