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LC-MS/MS를 이용한 농산물 중 Dimpropyridaz와 Cyclobutrifluram의 동시 시험법 개발 및 검증 KCI 등재

Development of a Simultaneous Analytical Method for Dimpropyridaz and Cyclobutrifluram in Agricultural Products using LC-MS/MS

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한국식품위생안전성학회지 (Journal of Food Hygiene and Safety)
한국식품위생안전성학회 (Korean Society of Food Hygiene and Safety)
초록

딤프로피리다즈는 pyrazole carboxamide 계열 살충제로 활성형은 TRPV 상류 부위를 표적으로 하여 신호전달을 차단하며 진딧물 등의 해충 방제에 효과적이다. 사이클로 뷰트리플루람은 phenethyl pyridineamide 계열 살충제로 미 토콘드리아 전자 수송 사슬복합체 II의 호흡작용을 저해 한다. 딤프로피리다즈와 사이클로뷰트리플루람에 대한 국 내 잔류물의 정의는 모화합물이며, 각각 수박, 호박잎 등 29품목에 대하여 0.03-7.0 mg/kg, 배추 등 6품목에 대하여 0.03 mg/kg으로 잔류허용기준이 설정되어 있다. 본 연구 에서는 농산물 중 딤프로피리다즈와 사이클로뷰트리플루람 의 잔류량을 분석하기 위한 공정시험법을 마련하고자 하였 다. 딤프로피리다즈 및 사이클로뷰트리플루람을 분석하기 위하여 아세토니트릴을 추출용매로 사용하는 QuEChERS법 을 이용하여 추출 및 정제조건을 확립한 후, LC-MS/MS 를 분석기기로 선정하였다. 딤프로피리다즈 및 사이클로 뷰트리플루람의 결정계수(R2)는 모두 0.99 이상으로 우수 하였으며, 정량한계는 0.01 mg/kg으로 나타났다. 대표 농 산물 5종(현미, 감자, 대두, 감귤, 고추)에 대하여 정량한 계, 정량한계 10배, 정량한계 50배 수준으로 처리하여 회 수율 실험을 한 결과 딤프로피리다즈의 평균 회수율은 85.5-101.5%, 사이클로뷰트리플루람은 86.8-108.5%을 보였 으며, 변이계수(coefficient of variation, CV)는 각각 10.9%, 13.7% 이하로 나타났다. 본 연구의 결과는 국제식품규격 위원회 농약 분석법 가이드라인25)의 잔류농약 분석 기준 및 식품의약품안전평가원의 식품 등 시험법 마련 표준절 차에 관한 가이드라인24)에 적합한 수준이다.

Dimpropyridaz, a pyrazole carboxamide insecticide, is highly effective for controlling pests such as locusts by targeting the transient receptor potential vanilloid (TRPV) upstream region and blocking signal transmission. Cyclobutyrifluram is a phenethyl pyridineamide insecticide that inhibits the respiratory action of the mitochondrial electron transport chain complex II. Establishing an official analysis method for safety management is required, as this drug is newly registered in Korea. Therefore, this study aimed to develop a residual analysis method for dimpropyridaz and cyclobutrifluram in five representative agricultural products. Dimpropyridaz and cyclobutrifluram were extracted using the EN method (a QuEChERS method) by comparing the recovery tests and matrix effects of the three quick, easy, cheap, effective, rugged and safe (QuEChERS) methods. Various sorbent agents have been used to establish clean-up methods. No differences were observed among the utilized sorbents. Therefore, MgSO4 and primary secondary amine (PSA) were selected as the final cleanup conditions. Liquid chromatography-mass spectrometry (LC-MS/MS) was used to analyze the selectivity and sensitivity of the target pesticide in the multiple reaction monitoring (MRM) mode. The results of the recovery test using the established analysis method for dimpropyridaz were 85.5-101.5% and for cyclobutrifluram were 86.8-108.5% and the coefficient of variation (CV) values were less than 10.9% and 13.7%, respectively. These results are consistent with the residue analysis criteria of the International Food Standards Committee and the guidelines of the Korea Food and Drug Administration.

목차
ABSTRACT
Materials and Methods
    시약 및 재료
    표준원액 및 표준용액의 조제
    추출 및 정제
    LC-MS/MS 분석조건
    시험법 유효성 검증
Results and Discussion
    추출 및 정제조건 확립
    기기분석조건 확립
    시험법 유효성 검증
    실험실간 검증
Acknowledgement
국문요약
Conflict of interests
ORCID
References
저자
  • 구선영(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Sun Young Gu (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 이수정(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Su Jung 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, Cheongju, Korea)
  • 박채영(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Chae Young 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, Cheongju, Korea)
  • 이정미(식품의약품안전처 식품의약품안전평가원 식품위해평가부 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, Cheongju, Korea) Corresponding author
  • 장귀현(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Gui Hyun Jang (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 엄미옥(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Miok Eom (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 정윤미(식품의약품안전처 광주지방식품의약품안전청 유해물질분석과) | Yun Mi Chung (Hazardous Substances Analysis Division, Gwangju Regional Food and Drug Administration, Gwangju, Korea)