한국식품위생안전성학회지 (Journal of Food Hygiene and Safety)

  • 제38권3호
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  • Pages.89-98
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  • 2023
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  • 1229-1153(pISSN)
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  • 2465-9223(eISSN)
한국식품위생안전성학회 (The Korean Society of Food Hygiene and Safety)
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가열증류법에 의한 식용유지의 잔류농약 분석법 개발

Residual Pesticide Analysis Method of Edible Oil via Heat Distillation Methods

  • 손미희 (경기도보건환경연구원 안산농수산물검사소) ;
  • 김재관 (경기도보건환경연구원 안산농수산물검사소) ;
  • 조영선 (경기도보건환경연구원 안산농수산물검사소) ;
  • 한나은 (경기도보건환경연구원 안산농수산물검사소) ;
  • 김병태 (경기도보건환경연구원 안산농수산물검사소) ;
  • 박명기 (경기도보건환경연구원 안산농수산물검사소) ;
  • 박용배 (경기도보건환경연구원 안산농수산물검사소)
  • 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)
  • 투고 : 2023.02.13
  • 심사 : 2023.06.10
  • 발행 : 2023.06.30
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초록

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.

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.

키워드

참고문헌

  1. Lim, J.K., Edible oil industry, Food Ind., 181, 10-37 (2004). 
  2. Lee, J.H., Park, J.M., Kim, H.J., Koh, J.H., Kim, J.M., Physicochemical changes in edible oils (soybean, canola, palm, and lard) and fried foods (pork cutlet and potato) depending on fry number. Kor. J. Food Sci. Technol. 49, 50-55 (2017).  https://doi.org/10.9721/KJFST.2017.49.1.50
  3. Lee, J.W., Park, J.W., Changes of fatty acid composition and oxidation stability of edible oils with frying number of french fried potatoes. J. Kor. Soc. Food Sci. Nut., 39, 1011-1017 (2010).  https://doi.org/10.3746/jkfn.2010.39.7.1011
  4. Kim, S., Policy of Reducing Benzopyrene in Foods, Food Ind. Nut., 19, 13-14 (2014). 
  5. Ministry of Food and Drug Safety, (2023, May 30). Korea Food Code. Retrieved from http://www.foodsafetykorea.go.kr/portal/safefoodlife/food/foodRvlv/foodRvlv.do 
  6. Kim, J.M., Method validation and measurement uncertainty for the simultaneous determination of synthetic phenolic antioxidants in edible oils. Master's thesis, Kangwon National University, Chuncheon, Korea (2017). 
  7. Nam, H.J., Seo, I.W., Lee, K.E., Lee, S.Y., Shin, H.S., Analysis of benzo[a]pyrene content in edible oils from Korean market. Food Eng. Prog., 13, 211-215 (2009). 
  8. Jang, M.R., Hong, M.S., Jung, S.Y., Choi, B.C., Lee, K.A., Kum, J.Y., Kim, I.Y., Kim, J.H., Chae, Y.Z., Analysis and risk assessment of benzo(a)pyrene in edible oils. J. Fd Hyg. Safety, 29, 141-145 (2014).  https://doi.org/10.13103/JFHS.2014.29.2.141
  9. Lee, M.J., Cho, M.K., Oh, S.H., Oh, C.H., Choi, D.S., Woo, J.W., Park, K.H., Jung, M.Y., Fatty acid composition, contents of tocopherols and phytosterols, and oxidative stability of mixed edible oil of perilla seed and rice bran oil. Korean J. Food & Nutr., 27, 59-65 (2014).  https://doi.org/10.9799/ksfan.2014.27.1.059
  10. Lee, M.G., Kim, J.S., Pesticide residues in chili pepper seeds and their transfer into the seed oil. Korean J. Food Sci. Technol., 48, 317-322 (2016).  https://doi.org/10.9721/KJFST.2016.48.4.317
  11. Lee, C.W., Shin, H.S., Removal of pesticide residues in rice bran oil by refining process. J. Food Hyg. Safety, 11, 89-97 (1996). 
  12. Muhamad, H., Abdullah, M.P., Ai, T.Y., Chian, S.S., Optimization of the sweep co-distillation clean-up method for the determination of organochlorine pesticide residues in palm oil. J. Oil palm res., 16, 3036 (2004). 
  13. Armishaw, P., Millar, R.G., Roderick G., Comparison of gel permeation hromatography, sweep codistillation, and florisil column adsorption chromatography as sample cleanup techniques for the determination of organochlorine pesticide residues in animal fats. J. AOAC Int., 76, 1317-1322 (1993).  https://doi.org/10.1093/jaoac/76.6.1317
  14. Luke, B.G., Richards, J.C., Recent advances in cleanup of fats by sweep co-distillation. Part 2. Organophosphorus residues, J. Assoc. Off. Anal. Chem., 67, 902-904 (1984). 
  15. Ministry of Food and Drug Safety, Analytical practices manual for pesticide residues in foods, 5th ed, MFDS, Cheongju, Koear, pp. 78-82 (2017). 
  16. Mum, S.K., Park, J.J., Kim, C.E., Kim, J.K., Kim, Y.H., Lee, K. C., Studies on the extraction methods and residual contents of pesticides in meats II. Organophosphorous pesticides. Kor. J. Vet. Publ. Hlth., 20, 241-248 (1996). 
  17. Kim, J.K., Whang, H.J., Oh, M.H., Do, Y.S., Yoon, M.H., Extraction method of antioxidants in soybean oil. (1999), Korean J. Food & Nutr., 12, 358-363 (1999). 
  18. Li, L., Zhang, H., Pan, C., Zhou, Z., Jiang, S., Liu, F., Multiresidue analytical method of pesticides in peanut oil using low-temperature cleanup and dispersive solid phase extraction by GC-MS. J. Sep. Sci., 30, 2097-2104 (2007).  https://doi.org/10.1002/jssc.200700052
  19. Li, L., Zhou, Z., Pan, C., Qian, C., Jiang, S., Liu, F., Determination of Organophosphorus pesticides in soybean oil, peanut oil and sesame oil by low-temperature extraction and GC-FPD. Chromatographia, 66, 625-629 (2007).  https://doi.org/10.1365/s10337-007-0349-9
  20. Liu, Y., Shen, D., Mo, R., Zhong, D., Tang, F., Simultaneous determination of 15 multiresidue organophosphorous pesticides in camellia oil by MSPD-GC-MS. Bull. Environ. Contam. Toxicol., 90, 274 -279, (2013).  https://doi.org/10.1007/s00128-012-0932-0
  21. Fuentes, E. Baez, M.E. Diaz, J., Microwave-assisted extraction at atmospheric pressure coupled to different cleanup methods for the determination of organophosphorus pesticides in olive and avocado oil. J. Chrom. A, 1216, 8859-8866 (2009).  https://doi.org/10.1016/j.chroma.2009.10.082
  22. He, Z., Wang Y., Wang, L., Peng, Y., Wang, W., Liu, X., Determination of 255 pesticides in edible vegetable oils using QuEChERS method and gas chromatography tandem mass spectrometry. Anal. Bio. Chem., 409, 1017- 1030, (2017).  https://doi.org/10.1007/s00216-016-0016-9
  23. Nguyen, T.D., Lee, M.H., Lee, G.H., Rapid determination of 95 pesticides in soybean oil using liquid-liquid extraction followed by centrifugation, freezing and dispersive solid phase extraction as cleanup steps and gas chromatography with mass spectrometric detection. Microchemical J., 95, 113-119 (2010).  https://doi.org/10.1016/j.microc.2009.11.009
  24. Sanchez, A.G., Martos, N.R., Ballesteros, E., Multiresidue analysis of pesticides in olive oil by gel permeation chromatography followed by gas chromatography-tandem mass-spectrometric determination. Anal. Chim. Acta., 558, 53-61 (2006).  https://doi.org/10.1016/j.aca.2005.11.019
  25. CAC (CODEX Alimentarius Commission), (2023, May 30). Guidelines on good laboratory practice in pesticide residue analysis CAC/GL 40-1993. Retrieved from https://www.fao.org/fao-who-codexalimentarius/codex-texts/guidelines/en/ 
  26. Ministry of Food and Drug Safety, (2023, May 30). Guidelines on standard procedures for preparing analysis method. Retrieved from http://www.nifds.go.kr/brd/m_15/view.do?seq=8215 
  27. The International Council for Harmonisation of Technical Requirements for Pharmaceuticals for Human Use (ICH), (2023, May 30). Validation of analytical procedures: Text and methodology Q2(R1). Retrieved from https://database.ich.org/sites/default/files/Q2_R1__Guideline.pdf 
  28. National Institute of Food and Drug Safety Evaluation, (2023, May 30). Guidelines for validation of analytical procedure for pharmaceuticals, etc. Retrieved from https://www.mfds.go.kr/docviewer/skin/doc.html?fn=ba6253f045c544ba75922c4dc9affaa7&rs=/docviewer/result/data0011/12697/1/202306