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LC/MS/MS를 이용한 식용란 중 fluoroquinolone계 항균물질의 분석법에 관한 연구

Study on analytical method of fluoroquinolone residues in eggs by LC/MS/MS

최유정
한국동물위생학회 (THE KOREAN SOCIETY OF VETERINARY SERVICE)|2007.03|한국동물위생학회지|제30권 제1호|pp. 13-21

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참고문헌

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초록

Abstract

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(pH7.4). The extract was cleaned up by passage though Oasis 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 AtlantisTM dC18 reversed-phase column(4.6×150㎜, 5㎛) 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 1Corresponding author Phone : +82-55-771-6641, Fax : +82-55-771-6619E-mail : cyj9144@hanmail.net product ion combinations of m/z 320 302, 332 314, 360 342 and m/z 358 340 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 0.1ppm 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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