Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Residual Pesticide Analysis Method of Edible Oil via Heat Distillation Methods

가열증류법에 의한 식용유지의 잔류농약 분석법 개발

  • Mi-Hui Son (Ansan Agricultural and Fishery Products Inspection Center) ;
  • Jae-Kwan Kim (Ansan Agricultural and Fishery Products Inspection Center) ;
  • Young-Seon Cho (Ansan Agricultural and Fishery Products Inspection Center) ;
  • Na-Eun Han (Ansan Agricultural and Fishery Products Inspection Center) ;
  • Byeong-Tae Kim (Ansan Agricultural and Fishery Products Inspection Center) ;
  • Myoung-Ki Park (Ansan Agricultural and Fishery Products Inspection Center) ;
  • Yong-Bae Park (Ansan Agricultural and Fishery Products Inspection Center)
  • 손미희 (경기도보건환경연구원 안산농수산물검사소) ;
  • 김재관 (경기도보건환경연구원 안산농수산물검사소) ;
  • 조영선 (경기도보건환경연구원 안산농수산물검사소) ;
  • 한나은 (경기도보건환경연구원 안산농수산물검사소) ;
  • 김병태 (경기도보건환경연구원 안산농수산물검사소) ;
  • 박명기 (경기도보건환경연구원 안산농수산물검사소) ;
  • 박용배 (경기도보건환경연구원 안산농수산물검사소)
  • Received : 2023.02.13
  • Accepted : 2023.06.10
  • Published : 2023.06.30
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Abstract

Currently, no guidelines exist regarding the maximum residues of pesticides in edible oil which is a processed food commonly consumed in Korea. This lack of guidelines hinders the evaluation of the safety of edible oil in terms of pesticide contamination. In this study, an analysis method based on heat distillation and GC-MS/MS was established by optimizing the extraction and purification procedure for 68 pesticides. Important variables in the thermal distillation procedure included heating temperature and time, and we found the nitrogen flow rate as a mobile phase and the type of dissolving solvent were not considerably affected. The determination coefficient (R2) of the residual pesticide was 0.99 or higher, and the quantitative limit (LOQ) was 0.01-0.02 mg/L. The average recovery rate (n=5) was 66.1-120.0% and the relative standard deviation was lower than ±10% when 68 pesticides were spiked at concentrations of 0.01-0.02, 0.1, and 0.5 mg/L. In addition, the within-laboratory precision was less than ±11%, meeting the Korea Food and Drug Safety Evaluation Institute's Guidelines on Standard Procedures for Preparing Food Testing Methods (2016). Therefore, the test method developed in this study can be used as a test method for managing the safety of the residual pesticide concentration in edible oil.

현재, 국내에서는 가공식품인 식용유지에 대한 잔류농약 허용기준이 설정되어 있지 않아 잔류농약은 식용유 품질평가의 사각지대라 할 수 있다. 본 연구에서는 식용유지에서 가열증류법을 이용하여 68종의 농약을 대상으로 추출 및 정제법을 최적화하여 GC-MS/MS 분석법을 확립하였다. 가열증류법은 가열온도 및 시간의 영향을 받았으며 이동상의 역할을 하는 질소의 유량과 용출용매의 종류에는 큰 영향을 받지 않는 것으로 나타났다. 본 연구에서 잔류농약의 결정계수(R2)는 0.99 이상으로 나타났고, 정량한계(LOQ)는 0.01-0.02 mg/L이었으며, 대두유를 이용하여 0.01, 0.02, 0.1, 0.5 mg/L 수준으로 회수율 실험 결과 평균 회수율(n=5)은 66.1-120.0%이었고 상대표준편차는 ±10%이하로 나타났다. 또한 실험실내 일간정밀도는 11%이하로 조사되어, 식품의약품안전평가원의 '식품등 시험법 마련 표준절차에 관한 가이드라인(2016)'에 적합한 수준임을 확인하였다. 따라서 본 연구에서 개발한 시험법은 식용유지의 잔류농약 안전관리를 위한 시험법으로 활용이 가능할 것으로 기대된다.

Keywords

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