본 연구는 농산물 중 잔류허용기준 신설 예정 농약 퀴 녹시펜의 공정시험법을 개발하기 위하여 수행되었다. 퀴녹시펜은 퀴놀린(quinoline) 계열의 표면이동성 살균제로써 흰가루병균(powdery mildew) 방제 효과가 있다. 퀴녹시펜 의 잔류물의 정의는 코덱스, 유럽, 일본의 경우 농산물과 축산물 대상으로 모화합물로, 미국의 경우 농산물 대상으로 모화합물로 설정되어 있다. 현재, 국내에서는 농산물 중 퀴녹시펜의 잔류물의 정의 및 잔류허용기준이 설정되어있지 않고, 수입식품 중 체리에 대한 잔류허용기준 신설이 최초 요청되었으며 국내 유통 농산물 중 잔류량에 대한 안전관리 확보를 위해 잔류물의 정의를 모화합물로 규정하 고 적부판정을 위한 공정시험법을 개발하고자 하였다. 퀴녹시펜의 물리·화학적 특성을 고려하여 QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe)법을 이용한 추출 및 정제법을 최적화하여 LC-MS/MS에 의한 분석법을 확립하였다. 퀴녹시펜의 결정계수(R2)는 0.99 이상으로 높은 직선성을 보여주었고, 퀴녹시펜의 시험법 정량한계 (LOQ)는 0.005 mg/kg이며, 대표 농산물 5종(현미, 감자, 대두, 감귤, 고추)에 대하여 1 LOQ (0.005 mg/kg), 10 LOQ (0.05 mg/kg), 50 LOQ (0.25 mg/kg) 수준으로 회수율 실험한 결과 평균 회수율(n=5)은 73.5-86.7%이었으며 상대표 준편차는 8.9%이하로 확인되었다. 또한 실험실간 검증 결과 두 실험실간 회수율 결과에 따른 평균값은 77.2-95.4% 이며 변이계수(CV) 또한 14.5% 이하로 조사되어, 본 연구는 국제식품규격위원회 가이드라인(Codex Alimentarius Commission, CAC/GL 40)의 잔류농약 분석 기준 및 식품 의약품안전평가원의 ‘식품등 시험법 마련 표준절차에 관한 가이드라인(2016)’에 적합한 수준임을 확인하였다. 따라서 본 연구에서 개발한 시험법은 농산물 중 잔류할 수 있는 퀴녹시펜의 안전관리를 위한 공정시험법으로 활용 가능할 것이다.

An analytical method was developed for the determination of quinoxyfen in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted with 1% acetic acid in acetonitrile and water was removed by liquid-liquid partitioning with MgSO4 (anhydrous magnesium sulfate) and sodium acetate. Dispersive solid-phase extraction (d-SPE) cleanup was carried out using MgSO4, PSA (primary secondary amine), C18 (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed by using LC-MS/MS in positive mode with MRM (multiple reaction monitoring). The matrix-matched calibration curves were constructed using six levels (0.001-0.25 μg/mL) and the coefficient of determination (R2) was above 0.99. Recovery results at three concentrations (LOQ, 10 LOQ, and 50 LOQ, n=5) were in the range of 73.5-86.7% with RSDs (relative standard deviations) of less than 8.9%. For inter-laboratory validation, the average recovery was 77.2-95.4% and the CV (coefficient of variation) was below 14.5%. All results were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for quinoxyfen determination in agricultural commodities. This study could be useful for the safe management of quinoxyfen residues in agricultural products.

ABSTRACT
 Materials and Methods
  시약 및 재료
  표준원액 및 표준용액의 조제
  추출 및 정제
  LC-MS/MS 분석조건
  시험법 검증
 Results and Discussion
  기기분석조건 확립
  추출 및 정제조건 확립
  시험법 검증
  실험실간 시험법 검증
 국문요약
 Reference

• 조성민(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Sung Min Cho (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
• 도정아(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Jung-Ah Do (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
• 이한솔(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Han Sol 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)
• 박지수(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Ji-Su 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)
• 신혜선(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Hye-Sun Shin (Pesticide and Veterinary Drug Residues Division, Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
• 장동은(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Dong Eun 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)
• 최영내(한국식품과학연구원) | Young-Nae Choi (Korea Advanced Food Research Institute)
• 정용현(식품의약품안전처 식품의약품안전평가원 식품위해평가부 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)
• 이강봉(식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) | Kangbong 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)