Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Simultaneous Determination of Aminoglycoside Antibiotics in Meat using Liquid Chromatography Tandem Mass Spectrometry

LC-MS/MS를 이용한 육류 중 아미노글리코사이드계 항생제 9종의 동시분석 및 적용성 검증

  • Cho, Yoon-Jae (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Choi, Sun-Ju (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Kim, Myeong-Ae (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Kim, MeeKyung (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Yoon, Su-Jin (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Chang, Moon-Ik (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Lee, Sang-Mok (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Kim, Hee-Jeong (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Jeong, Jiyoon (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Rhee, Gyu-Seek (Pesticide and Veterinary Drug Residues Division, National Institute of Food & Drug Safety Evaluation) ;
  • Lee, Sang-Jae (Food Safety Evaluation Department, National Institute of Food & Drug Safety Evaluation)
  • 조윤제 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 최선주 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김명애 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김미경 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 윤수진 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 장문익 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이상목 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김희정 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 정지윤 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이규식 (식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이상재 (식품의약품안전평가원 식품위해평가부)
  • Received : 2014.02.12
  • Accepted : 2014.05.14
  • Published : 2014.06.30
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Abstract

A simultaneous determination was developed for 9 aminoglycoside antibiotics (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygromycin B, kanamycin, neomycin, spectinomycin, and streptomycin) in meat by liquid chromatography tandem mass spectrometry (LC-MS/MS). Each parameter was established by multiple reaction monitoring in positive ion mode. The developed method was validated for specificity, linearity, accuracy, and precision based on CODEX validation guideline. Linearity was over 0.98 with calibration curves of the mixed standards. Recovery of 9 aminoglycosides ranged on 60.5~114% for beef, 60.1~112% for pork and 63.8~131% for chicken. The limit of detection (LOD) and limit of quantification (LOQ) were 0.001~0.009 mg/kg and 0.006~0.03 mg/kg, respectively in livestock products including beef, pork and chicken. This study also performed survey of residual aminoglycoside antibiotics for 193 samples of beef, pork and chicken collected from 9 cities in Korea. Aminoglycosides were not found in any of the samples.

LC-MS/MS를 이용하여 아미노글리코사이드계 동물용의 약품 9종에 대하여 동시분석법을 확립하고 잔류실태조사를 수행하였다. 현재 식품공전에 수록된 시험법을 기본으로 분석법을 개선하였으며 국제식품규격위원회 기준에 따라 특이성, 직선성, 정확성, 정밀성, 정량한계 등을 검증하였다. 아미노글리코사이드 혼합표준용액을 잔류허용기준의 0.125배, 0.25, 0.5, 1, 2, 4배 농도에 따라 검량선을 작성한 결과 0.98 이상의 직선성을 확인하였다. 소고기의 회수율은 60.5~114%, 돼지고기의 회수율은 60.1~112%, 닭고기 회수율은 63.8~131%을 나타내었다. 또한 LOD는 0.001~0.009 mg/kg, LOQ는 0.006~0.03 mg/kg이었다. 국내유통 중인 축산물 (소고기, 돼지고기, 닭고기) 193건을 수거하여 개선된 분석법의 적용성 검증과 축산물의 안전성 확인을 위한 잔류조사를 수행한 결과 시험법의 적용성이 충분히 검증되었으며 모든 시료에서 아미노글리코사이드 계열의 항생제가 검출되지 않아 유통 축산물이 안전한 것으로 확인되었다. 확립된 분석법은 식육에 잔류할 수 있는 아미노글리코사이드계열 동물용의약품 안전관리에 활용할 수 있을 것으로 사료되는 바이다.

Keywords

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