Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Analysis of residual neomycin in honey by LC-MS/MS

LC-MS/MS에 의한 벌꿀 중 잔류 네오마이신의 분석

  • 심영은 (경기대학교 자연과학대학 화학과) ;
  • 정지윤 (식품의약품안전청 식품잔류약품과) ;
  • 명승운 (경기대학교 자연과학대학 화학과)
  • Received : 2009.02.02
  • Accepted : 2009.07.03
  • Published : 2009.08.25
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Abstract

An effective and specific procedure for confirmation of neomycin, aminoglycoside antibiotic in honey was developed and validated. Honey was adjusted to pH 2 with 0.1M HCl and applied to weak cation-exchange SPE cartridge. Neomycin was eluted with basified methanol. Following separation by ion-pairing liquid chromatography, neomycin was analysed with positive electrospray ionization and MRM mode. Quantification was linear over the range of $5.0{\sim}250.0{\mu}g/kg$ ($r^2$ >0.9951). The precision (R.S.D.) and accuracy (as a bias) of quality control samples in honey ranged 11.5~18.7% and 10.9~20.9%, respectively. Established method can be applied to analysis of neomycin in honey.

벌꿀 중에 잔류하는 아미노그라이코사이드 항생제인 네오마이신을 효과적으로 분석하는 방법을 개발하고 방법에 대한 유효성 검증을 수행하였다. 0.1M 염산을 사용하여 벌꿀의 pH를 2로 조절한 후 고체상 추출(SPE) 고체상인 양이온교환 카트리지에 적재한 후 염기성 메탄올로 용리하였다. 용리된 추출물은 이온쌍 시약을 사용한 이온쌍 크로마토그래피법으로 분리한 후 LC/(+)ESI-MS/MS의 MRM 방법으로 분석하였다. 정량분석을 위해서 spike 한 $5.0{\sim}250{\mu}g/kg$ 농도 범위에서 검정곡선은 좋은 직선성 ($r^2$ > 0.9951)을 나타내었다. 분석방법의 상대표준편차는 11.5~18.7%이었고 정확도는 bias로 10.9~20.9%이었다. 확립된 분석방법은 벌꿀 중에서 네오마이신의 분석방법으로 유용하게 사용될 수 있을 것이다.

Keywords

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