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GC-ECD를 이용한 flutianil 잔류량 분석법 개발 및 확인

Development and Validation of an Analytical Method for Flutianil Residue Identification Using Gas Chromatography-Electron Capture Detection

  • 권지은 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 도정아 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 박혜진 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 이지영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 조윤제 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 오재호 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 이상재 (식품의약품안전처 식품의약품안전평가원 식품위해평가부) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 식품위해평가부)
  • Kwon, Ji-Eun (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Do, Jung-Ah (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Park, Hyejin (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Lee, Ji-Young (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Cho, Yoon-Jae (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Oh, Jae-Ho (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Rhee, Gyu-Seek (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Lee, Sang-Jae (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS) ;
  • Chang, Moon-Ik (Food Safety Evaluation Department, National Institute of Food and Drug Safety Evaluation, MFDS)
  • 투고 : 2013.07.02
  • 심사 : 2013.11.14
  • 발행 : 2014.02.28

초록

Flutianil은 흰가루병에 높은 방제효과를 가지는 thiazolidine계 살균제로서 고추, 피망, 오이, 참외에 대해 flutianil의 사용등록이 신청됨에 따라 농산물 중 flutianil 잔류량을 측정하기 위한 검사법을 개발하였다. Flutianil 잔류물은 acetonitrile로 추출하여 포화식염수와 dichloromethane을 이용한 액-액분배과정을 수행하였고, silica 카트리지를 이용하여 clean-up을 실시한 후 GC-ECD를 통해 기기분석을 수행하였으며, GC-MS로 재확인하였다. flutianil 표준품의 직선성은 상관계수($R^2$)가 0.999이상으로 우수하였고 고추, 피망, 감귤, 감자, 현미, 대두에 대한 flutianil의 회수율을 측정한 결과, 76.5-108.0%의 범위로 10% 미만의 표준오차를 나타내었으며, 분석법의 검출한계는 0.004 mg/kg, 정량한계 0.02 mg/kg이었다. 이는 코덱스 가이드라인(CAC/GL 40)인 회수율 70-120%, 분석오차 10 미만에 적합함을 보여주어 분석법의 정확성을 확인하였다. 본 연구에서 개발한 시험법은 flutianil 분석을 위한 신속, 정확한 시험법으로, 국내에서 유통되는 농산물 중 flutianil 잔류물의 안전관리를 위한 공정시험법으로 활용될 예정이다.

A sensitive and simple analytical method to identify flutianil residues in agricultural commodities was developed and validated using gas chromatography-electron capture detection (GC-ECD) and mass spectrometry (GC-MS). The flutianil residues were extracted with acetonitrile, partitioned with dichloromethane, and then purified using a silica solid-phase extraction (SPE) cartridge. The method was validated using pepper, sweet pepper, mandarin, hulled rice, soybean, and potato spiked with 0.02 or 0.2 mg/kg flutianil. The average recovery of flutianil was 76.5-108.0% with a relative standard deviation of less than 10%. The limit of detection and limit of quantification were 0.004 and 0.02 mg/kg, respectively. The result of recoveries and relative standard deviation were in line with Codex Alimentarius Commission Guidelines (CAC/GL 40). These results show that the method developed in this study is appropriate for flutianil identification and can be used to maintain the safety of agricultural products containing flutianil residues.

키워드

참고문헌

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피인용 문헌

  1. Monitoring and Risk Assessment of Pesticide Residues in Commercial Environment-Friendly Agricultural Products Distributed Using LC-MS/MS in Seoul Metropolitan Area vol.47, pp.3, 2015, https://doi.org/10.9721/KJFST.2015.47.3.306
  2. sequential hydrolysis/rearrangement reactions of 5-arylidenethiazolidin-4-ones at room temperature vol.16, pp.11, 2018, https://doi.org/10.1039/C7OB02924A