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Development and Validation of an Official Analytical Method for Determination of Ipfencarbazone in Agricultural Products using GC-ECD

GC-ECD를 이용한 농산물 중 Ipfencarbazone의 신규분석법 개발 및 검증

  • Jang, Jin (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Department of Food Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Heejung (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Department of Food Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Lee, Eun-Hyang (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Department of Food Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Ko, Ah-Young (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Department of Food Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Ju, Yunji (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Department of Food Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kim, Sooyeon (Hazardous Substances Analysis Division, Center for Food and Drug Analysis, Gyeongin regional Korea Food and Drug Administration) ;
  • Chang, Moon-Ik (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Department of Food Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Rhee, Gyu-Seek (Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Department of Food Safety Evaluation, Ministry of Food and Drug Safety)
  • 장진 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김희정 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이은향 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 고아영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 주윤지 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김수연 (경인지방식품의약품안전청 시험분석센터 유해물질분석과) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2015.07.03
  • Accepted : 2015.09.11
  • Published : 2015.09.30

Abstract

Ipfencarbazone is a herbicide of the tetrazolinone class, and is believed to be an inhibitor of very long chain fatty acids (VLCFAs), which control cell division in weeds. The objective of this study was to develop and validate an official analytical method for ipfencarbazone determination in agricultural products. The ipfencarbazone residues in agricultural products were extracted with acetone, partitioned with n-hexane, and then purified through silica SPE cartridge. Finally, the analyte was quantified by gas chromatograph-electron capture detector (GC-ECD) and confirmed with gas chromatograph/mass spectrometer(GC/MS). The linear range of ipfencarbazone was 0.01 to 1.0 mg/L with the coefficient of determination ($r^2$) of 0.9999. The limit of detection (LOD) and quantification (LOQ) was 0.003 and 0.01 mg/kg, respectively. In addition, average recoveries of ipfencarbazone ranged from 80.6% to 112.3% at the different concentration levels LOQ, 10LOQ and 50LOQ, while the relative standard deviation was 2.2-8.6%. All values were consistent with the criteria ranges requested in the CODEX guidelines. Furthermore, and inter-laboratory study was conducted to validate the method. This proposed method for determination of ipfencarbazone residues in agricultural products can be used as an official analytical method.

Ipfencarbazone은 tetrazolinone계 화합물로 잡초 세포막의 주성분인 장쇄지방산(VLCFAs) 합성을 억제하여 세포 분열을 저해하는 작용을 하는 제초제이다. 본 연구에서는 국내 신규농약 ipfencarbazone에 대한 안전관리를 위해 농산물 중 ipfencarbazone의 잔류분석법을 개발하였다. 농산물 시료(현미, 대두, 고추, 감귤, 감자) 중 ipfencarbazone을 acetone으로 추출한 뒤 n-hexane을 이용해 분배하고 silica SPE 카트리지를 통한 흡착크로마토그래피법을 이용해 정제하였다. 이를 GC-ECD를 이용해 분석해 정량평가를 하였으며, 재확인을 위해 GC/MS로 분석하였다. 분석법의 직선성은 농도 대비 피크면적과의 결정계수($r^2$)가 0.999 이상으로 우수하였으며, 검출한계 및 정량한계는 각각 0.003, 0.01 mg/kg으로 높은 감도를 나타냈다. 농산물 시료 중 모든 처리구에서 평균 회수율은 80.6%-112.3%(RSD 10% 이내)였고, 경인청과의 실험실간 검증결과에서도 95.1-106.1%를 나타냈다. 모든 결과를 종합해볼 때 개발된 분석법은 모두 CODEX 가이드라인(CAC/GL 40, 2003)의 기준이내를 만족하는 값으로 확인되었다. 따라서 개발된 분석법의 낮은 검출한계 및 정량한계, 우수한 직선성, 회수율 시험을 통한 양호한 정밀성 및 재현성 등을 종합해볼 때 이는 농산물 중 ipfencarbazone을 분석하기 위한 공정분석법으로 사용되기에 적합할 것으로 판단된다.

Keywords

References

  1. CAC (CODEX Alimentarius Commission) (2003) Guidelines on good laboratory practice in residue analysis, CAC/GL 40-1993, Rev.1-2003, Rome, Italy.
  2. EFSA (European Food Safety Authority) (2014) http://www.efsa.europa.eu/fr/efsajournal/doc/3737.pdf
  3. Hokko 화학공업주식회사 (2013) 농약초록(일반명: Ipfencarbazone). http://www.acis.famic.go.jp/syouroku/ipfencarbazone/ipfencarbazone_01.pdf
  4. Hubert Menne and Helmut Kocher (2008) HRAC Classification of Herbicides and Resistance Development, Modern crop protection compounds 3:5-24.
  5. Jane Elisabeth Corbin, Christopher John Mathews, Glynn Mitchell, Claudio Screpanti (2013) Novel herbicide, United states patent application publication. PCT/GB10/02268 http://images3.freshpatents.com/pdf/US20130252811A1.pdf
  6. MHLW (Ministry of Health, Labour and Welfare) (2014) http://www.m5.ws001.squarestart.ne.jp/foundation/agrdtl.php?a_inq=7550
  7. Sun Qixia, Jang Yifei, Li Youshun, Wang Shengxiang, Chen Qian. (2012) Analysis of ipfencarbazone in 2.5% GR by HPLC, Pesticide Science and Administration, 12:50-52.
  8. 동방아그로 (2012) Benzobicyclon+mazosulfuron+Ipfencarbazone SC 중 ipfencarbazone의 작물 (벼) 잔류성 시험 보고서
  9. 동방아그로 (2013) 원제초록: ipfencarbazone
  10. 일본 약사.식품 위생 심의회 (2013) Ipfencarbazone에 따른 식품 규격(식품 중 농약 잔류기준 설정)의 설정. http://www.mhlw.go.jp/shingi/2004/04/dl/s0420-4-t17.pdf