• 농약과학회지
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• 제2권3호
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• pp.79-84
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• 1998

콩나물중 carbendazim 잔류분을 정량하고 확인할 수 있는 새로운 분석법을 확립하고자 tandem HPLC(UV & FL) 및 APcI를 source로 사용한 LC/MS를 이용하였다. 이를 위해 FL(fluorescence) 검출기를 UV(ultraviolet) 검출기와 나란히 연결하여 UV 검출기의 경우 280 nm 파장을 그리고 FL 검출기의 경우는 excitation파장과 emission파장을 각각 280 mn와 310 nm로 설정하였다. 분석결과 carbendazim의 검출한계는 $0.04{\mu}g/kg$이었다. 콩나물에 carbendazim을 0.5, 1.0 및 2.0 ppm 수준으로 첨가하여 회수율을 측정한 결과 그 평균값은 89.1%이었다. APcI source를 사용한 LC/MS 질량스펙트럼 방법은 콩나물중 carbendazim 잔류분을 최종 확인할 수 있었다. APcI LC/MS 방법은 전자충격에 의한 질량스펙트럼에 비해 훨씬 간단한 fragment를 형성할 뿐 만 아니라 carbendazim의 경우 m/z 133, m/z 159, m/z 191($M^{+}$)의 전형적인 fragment 이온을 형성하므로, 이 방법을 병행한다면 콩나물중 carbendazim 잔류분을 효과적으로 확인할 수 있을 것으로 사료되었다.

• 한국동물위생학회지
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• 제30권1호
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• pp.13-21
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• 2007

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 $Oasis^{(R)}$ 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 $Atlantis^{TM}$ $dC_{18}$ reversed-phase column ($4.6{\times}150mm,\;5{\mu}m$) 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 $320\;{\dashrightarrow}\;302,\;332\;{\dashrightarrow}\;314,\;360\;{\dashrightarrow}\;342$ and m/z $358\;{\dashrightarrow}\;340$ 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 0.1 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.