Korean Journal of Food Science and Technology (한국식품과학회지)

Korean Society of Food Science and Technology (한국식품과학회)
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Analysis and Uncertainty Estimation of Zearalenone in Cereal-Based Products by LC-MS/MS

LC-MS/MS를 이용한 곡류가공품의 제랄레논 분석과 측정불확도 추정

  • Choi, Eun Jung (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kang, Sung Tae (Department of Food Science and Technology, Seoul National University of Science and Technology) ;
  • Jung, So Young (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Shin, Jae Min (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Jang, Min Su (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Lee, Sang Me (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Kim, Jung Hun (Seoul Metropolitan Government Research Institute of Public Health and Environment) ;
  • Chae, Young Zoo (Seoul Metropolitan Government Research Institute of Public Health and Environment)
  • 최은정 (서울시보건환경연구원) ;
  • 강성태 (서울과학기술대학교 식품공학과) ;
  • 정소영 (서울시보건환경연구원) ;
  • 신재민 (서울시보건환경연구원) ;
  • 장민수 (서울시보건환경연구원) ;
  • 이상미 (서울시보건환경연구원) ;
  • 김정헌 (서울시보건환경연구원) ;
  • 채영주 (서울시보건환경연구원)
  • Received : 2012.06.21
  • Accepted : 2012.10.15
  • Published : 2012.12.31
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Abstract

A survey of zearalenone contamination was conducted on cereal-based products by using an immunoaffinity column with LC-MS/MS. The calibration curve showed good lineality, with correlation coefficients ($R^2$) of 0.999 in the concentration range from 1 to 250 ng/mL. The limits of detection and quantification were approximately $0.3{\mu}g/kg$ and $1.0{\mu}g/kg$, respectively. The recoveries in the barley tea, Misutgaru and snack ranged from 73.6-107.8%. Zearalenone was detected in 10 samples (11.2% incidence). The highest zearalenone contamination level was $29.7{\mu}g/kg$ in the Misutgaru. This survey was conducted with uncertainty of measurement. The expanded uncertainty for zearalenone was estimated to be $44.9{\pm}5.0{\mu}g/kg$ (k=2, 95% confidence level) and $128.7{\pm}7.9{\mu}g/kg$ (k=2, 95% confidence level) for barley tea, $30.7{\pm}5.8{\mu}g/kg$ (k=2, 95% confidence level) and $173.7{\pm}14.9{\mu}g/kg$ (k=2.26, 95% confidence level) for Misutgaru, and $37.2{\pm}7.4{\mu}g/kg$ (k=2.31, 95% confidence level) and $151.0{\pm}10.4{\mu}g/kg$ (k=2, 95% confidence level) snack at the level of $41.7{\mu}g/kg$ and $166.7{\mu}g/kg$, respectively.

본 연구는 시중 유통되고 있는 곡류가공품 중 zearalenone을 immunoaffinity column 및 LC-MS/MS를 이용해 분석하였다. 표준용액의 검량선은 1, 10, 50, 100, 250 ng/mL농도 범위에서 상관계수($r^2$) 0.999 이상으로 양호한 직선성을 보였고, 검출한계 및 정량한계는 각각 0.3, $1.0{\mu}g/kg$이었다. 회수율은 77.2-107.8%였고, RSD는 1.5-12.8이었다. Product ion 283 m/z으로 정량하여 분석한 결과 과자류 21건 중 1건(4.8%) $2.3{\mu}g/kg$, 옥수수가공품 9건 중 2건(22.2%) $1.6-8.5{\mu}g/kg$, 기타곡류가공품 14건 중 선식 1건(7.1%)에서 $3.4{\mu}g/kg$이 검출되었다. 미숫가루가 19건 중 6건(31.6%)이 검출되어, 최고 검출율을 나타냈으며, $1.1-29.7{\mu}g/kg$의 검출농도를 나타내어 다른 곡류가공품에 비해 높은 수준이었다. 총 시료 89건 중 10건에서 제랄레논이 검출되어 11.2%의 검출율을 보였고, 오염수준은 $1.1-29.7{\mu}g/kg$이었다. 검출시료 12건은 product ion 187 m/z으로 모두 제랄레논임을 확인하였다. 제랄레논을 측정하는 과정 중 불확도 인자를 파악하여 측정 불확도를 추정 한 결과 41.7, $166.7{\mu}g/kg$일때 보리차는 각각 $44.9{\pm}5.0{\mu}g/kg$(95% 신뢰수준 약 k=2), $128.7{\pm}7.9{\mu}g/kg$(95% 신뢰수준 약 k=2), 미숫가루는 각각 $30.7{\pm}5.8{\mu}g/kg$(95% 신뢰수준 약 k=2), $173.7{\pm}14.9{\mu}g/kg$(95% 신뢰수준 k=2.26), 과자는 $37.2{\pm}7.4{\mu}g/kg$(95% 신뢰수준 k=2.31), $151.0{\pm}10.4{\mu}g/kg$(95% 신뢰수준 약 k=2)를 나타내었다.

Keywords

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