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Monitoring of Malachite Green in Freshwater Fish using LC-MS/MS

LC-MS/MS를 이용한 담수 어류 중 말라카이트 그린 분석

  • Choi, Hee-jin (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Yuk, Dong-Hyun (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Park, Young-Ae (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Jung, Bo-Kyeng (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Hong, Mi-Sun (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Yoon, Yong-Tae (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Yi, Hye-Jin (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Youn-Cheon (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Park, Sung-Kyu (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Moo-Sang (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Jung, Kweon (Gangnam Agro-marine Products Inspection Center, Seoul Metropolitan Government Research Institute of Public Health and Environment)
  • 최희진 (서울시보건환경연구원 강남농수산물검사소) ;
  • 육동현 (서울시보건환경연구원 강남농수산물검사소) ;
  • 박영애 (서울시보건환경연구원 강남농수산물검사소) ;
  • 정보경 (서울시보건환경연구원 강남농수산물검사소) ;
  • 홍미선 (서울시보건환경연구원 강남농수산물검사소) ;
  • 윤용태 (서울시보건환경연구원 강남농수산물검사소) ;
  • 이혜진 (서울시보건환경연구원 강남농수산물검사소) ;
  • 김연천 (서울시보건환경연구원 강남농수산물검사소) ;
  • 박성규 (서울시보건환경연구원 강남농수산물검사소) ;
  • 김무상 (서울시보건환경연구원 강남농수산물검사소) ;
  • 정권 (서울시보건환경연구원 강남농수산물검사소)
  • Received : 2015.10.20
  • Accepted : 2016.02.02
  • Published : 2016.02.28

Abstract

Malachite green was measured in 200 freshwater fish collected from local markets in Seoul using HPLC-DAD and LC-MS/MS. LC-MS/MS method was validated by linearity, accuracy, precision and limits of detection and quantification according to the CODEX's recommendation and HPLC-DAD method was applied according to the Food Code. Malachite green levels above the quantification limit of the LC-MS/MS were determined 18.5% (37) but just 1 fish was shown to contain malachite green by HPLC-DAD. Of 83 domestic fish, 21 fish were detected malachite green (25.3%). Of 117 fish from China, just 16 fish were detected malachite green (13.4%). In detection rate by species carp (35.0%), Crucian carp (30.4%), cat fish (28.0%), Korean bull head (23.8%), snake head (20.0%), eel (10.5%) and loach (7.8%) were in order. Especially, fish collected at summer were shown to contain malachite green frequently; the detection rate was 54.8%.

LC-MS/MS를 이용한 말라카이트 그린 유효성 검증결과 결정계수($R^2$)가 0.9996이상으로 높은 직선성을 보여주었으며 회수율은 어종에 따라 69.8%에서 93.9%범위를 보였다. 검출한계는 $0.013{\mu}g/kg$, 정량한계는 $0.038{\mu}g/kg$으로 CODEX의 가이드라인을 만족하였다. 수거된 어류 200건에서 말라카이트 그린을 분석한 결과, HPLC-DAD로는 1건이 검출되었으나, LC-MS/MS로 분석시 검출률은 18.5%였다. 본 연구 결과, LC-MS/MS를 이용한 말라카이트 그린 분석법이 우리나라에서 많이 소비되는 담수어종에서 분석에 적합하며, 1건을 제외한 모든 시료에서 식품공전의 잔류허용기준 이하로 말라카이트 그린이 검출되어서 안전한 것으로 나타났다. 다만 식품공전의 검출한계 이하로 말라카이트 그린이 검출되는 빈도가 18.5%임을 볼 때, 지속적으로 감시하고 모니터링 할 필요가 있음을 시사한다.

Keywords

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