Fluoroimide는 감과 감자의 둥근무늬낙엽병과 역병을 억제하는데 효과가있는 살진균제로서, 이전 사용되었던 fluoroimide의 시험법은 전처리시 발암물질인 benzene을 사 용하는 문제가 있었으며, 복잡한 시험법으로 인해 시간이 오래걸리고 효율이 떨어지는 단점이 있었다. 또한, fluoroimide 의 특성상 산성에서 안정한 편이므로 전처리 시 이를 고려해야 하는 문제가 있었으며, PLS시행에 따라 기존의 정량한계인 0.05 mg/kg보다 낮은 정량한계 요구로 인해 fluoroimide에 대한 새로운 전처리방법이 필요하였다. Fluoroimide가 산성에서 안정한 특성을 고려하여, 추출 시 4N의 염산을 사용하였고 용매는 acetic acid가 포함된 acetonitrile을 사용하였으며, MgSO4와 NaCl을 통해 추출하였다. 정제는 C18 (Octadecylsilane)과 GCB (graphitized carbon black)를 첨가하여 정제하였으며, 기기분석은 LCMS/ MS로 분석하였다. 대표농산물 5종(현미, 감자, 대두, 감귤, 고추)을 대상으로 정량한계(0.01 mg/kg), 정량한계 10배(0.1 mg/kg), 정량한계 50배(0.5 mg/kg)의 수준으로 회수율 실험을 5반복 실시하였으며, 그 결과는 농산물 5종에 서 85.7-106.9%의 회수율을 확인하였으며, 분석오차는 15.6% 이하의 결과를 보여, 국제식품 규격위원회 가이드 라인의 잔류농약 분석 기준 및 ‘식품등 시험법 마련 표준 절차에 관한 가이드라인(2016)’에 부합하였다. 상기의 결과를 통해 개선한 fluoroimide의 시험법은 benzene을 대체 해 실험자의 안전성을 확보하였고, QuEChERS법을 적용하여 효율을 높여, 안전관리에 대한 공정시험법으로서 활용가능할 것으로 사료된다.

Fluoroimide is a fungicide and is also used as a pesticide for persimmons and potatoes. The established fluoroimide pesticide analysis method takes a long time to perform and uses benzene, a carcinogen. In addition, a lower limit of quantification is required due to enforcement of the Positive List System. Therefore, this study aimed to improve the analysis method for residual fluoroimide to resolve the problems associated with the current method. The analytical method was improved with reference to the increased stability of fluoroimide under acidic conditions. Fluoroimide was extracted under acidic conditions by hydrogen chloride (4 N) and acetic acid. MgSO4 and NaCl were used with acetonitrile. C18 (octadecylsilane) 500 mg and graphitized carbon black 40 mg were used in the purification process. The experiment was conducted with agricultural products (hulled rice, potato, soybean, mandarin, green pepper), and liquid chromatograph-tandem mass spectrometry was used for the instrumental analysis. Recovery of fluoroimide was 85.7-106.9% with relative standard deviations (RSDs) of less than 15.6%. This study reports an improved method for the analysis of fluoroimide that might contribute to safety by substituting the use of benzene, a harmful solvent. Furthermore, the use of QuEChERS increased the efficiency of the improved method. Finally, this research confirmed the precise limit of quantification and these results could be used to improve the analysis of other residual pesticides in agricultural products.

ABSTRACT
Materials and Methods
    농약 및 시약
    추출 및 정제
    기기 분석
    시험법의 유효성 검증
Results and Discussion
    추출 정제과정 최적화
    기기분석조건 확립
    직선성 확인
    Fluoroimide의 회수율 확인
국문요약
References

• 김남영(식품의약품안전처 식품의약품안전평가원 잔류물질과) | Nam Young Kim (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
• 박은지(식품의약품안전처 식품의약품안전평가원 잔류물질과) | Eun-Ji Park (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
• 심재한(전남대학교 농업생명과학대학 농식품생명화학부) | Jae-Han Shim (Division of Applied Bioscience and Biotechnology College of Agriculture and Life Sciences, Chonnam National University)
• 이정미(식품의약품안전처 식품의약품안전평가원 잔류물질과) | Jung Mi Lee (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) Correspondence to
• 정용현(식품의약품안전처 식품의약품안전평가원 잔류물질과) | Yong Hyun Jung (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
• 오재호(식품의약품안전처 식품의약품안전평가원 잔류물질과) | Jae-Ho Oh (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)