Analysis of clenbuterol in bovine muscle and milk by LC-ESI/MS/MS

LC-ESI/MS/MS를 이용한 소고기와 우유에서의 클렌부테롤 분석

  • Hong, Selyung (Pesticide & Veterinary Drug Residues Division, Korea Food & Drug Administration) ;
  • Jeong, Jiyoon (Pesticide & Veterinary Drug Residues Division, Korea Food & Drug Administration) ;
  • Park, Hyejin (Pesticide & Veterinary Drug Residues Division, Korea Food & Drug Administration) ;
  • Lee, Soonho (Pesticide & Veterinary Drug Residues Division, Korea Food & Drug Administration) ;
  • Lee, Jongok (Pesticide & Veterinary Drug Residues Division, Korea Food & Drug Administration)
  • 홍세령 (식품의약품안전청, 식품잔류약품과) ;
  • 정지윤 (식품의약품안전청, 식품잔류약품과) ;
  • 박혜진 (식품의약품안전청, 식품잔류약품과) ;
  • 이순호 (식품의약품안전청, 식품잔류약품과) ;
  • 이종옥 (식품의약품안전청, 식품잔류약품과)
  • Received : 2008.10.31
  • Accepted : 2008.12.08
  • Published : 2008.12.25

Abstract

A liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS) method was developed for the determination and confirmation of clenbuterol in bovine muscle and milk. Clenbuterol and clenbuterol-D9 using as an internal standard in samples were extracted with ethyl acetate after hydrolysis and evaporated to dryness. The extracts were dissolved in 20% methanol and cleaned using HLB solid-phase extraction cartridge. The analytes were detected by LC-ESI/MS/MS on a $C_{18}$ column. Mass spectral acquisition was done in selected reaction monitoring (SRM) in positive ion mode to provide a high degree of sensitivity. Using MS/MS with SRM mode, the transitions (precursor to product) monitored were m/z 277${\rightarrow}$203 for clenbuterol, and m/z 286${\rightarrow}$204 for internal standard. The limits of quantitation (LOQ) and mean recoveries of clenbuterol in bovine muscle were $0.2{\mu}g/kg$ and 84.3~91.1%, respectively. The LOQ and mean recoveries in milk were $0.05{\mu}g/kg$ and 87.7~98.3%, respectively.

Keywords

clenbuterol;LC-ESI/MS/MS;bovine muscle;milk

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