The Korean Journal of Pesticide Science (농약과학회지)

The Korean Society of Pesticide Science (한국농약과학회)
권호 표지
DOI QR코드

DOI QR Code

Development of an Official Analytical Method for Determination of Imazapyr in Agricultural Commodities using HPLC-UVD

HPLC-UVD를 이용한 농산물 중 Imazapyr의 공정분석법 확립

  • 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) ;
  • 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) ;
  • 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) ;
  • Joo, Yoon Ji (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, Jinhong (Hazardous Substances Analysis Division, Center for Food and Drug Analysis, Daejeon 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) ;
  • 고아영 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이은향 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 주윤지 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 김진홍 (대전지방식품의약품안전청 유해물질분석과) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과) ;
  • 이규식 (식품의약품안전처 식품의약품안전평가원 식품위해평가부 잔류물질과)
  • Received : 2015.01.19
  • Accepted : 2015.03.18
  • Published : 2015.03.31
Download PDF
⟨ Previous Next ⟩

Abstract

A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

농산물 중 잔류농약의 안전관리를 위해 2014년 신규 기준설정 농약인 imazapyr의 분석법을 개발하였고 분석법의 정확성, 재현성, 정밀성, 선택성, 직선성에 대한 검증을 통하여 잔류농약 분석을 위한 공정분석법으로서의 유효성을 검증하였다. Imazapyr는 imidazolinone계 화합물로 아미노산의 생성을 억제하여 잡초의 생장을 방제하는 제초제이다. Imazapyr는 CODEX를 포함한 미국, 일본 등에서 잔류허용기준(MRL)이 설정되어 있으며, 우리나라에서도 대두에 대해 잔류허용기준을 설정할 예정이다. 비록 기준은 대두에 우선 설정되지만 농산물 전반에 대한 안전관리를 위해 곡류, 콩류, 채소류, 과일류, 서류에 대한 분석법를 개발하였고, 각 농산물군의 대표작물인 대두, 고추, 감귤, 현미, 감자 시료에 대해 분석법을 개발하였다. 시료 중 imazapyr를 methanol을 이용해 추출하고 dichloromethane으로 액-액 분배하여 극성 간섭물질을 제거하였으며, 현미 및 대두 등 유지시료의 경우 n-hexane/acetonitrile 분배법을 적용하여 유지성분을 추가로 제거하였다. 분석기기로는 Imazapyr의 낮은 증기압과 UV 파장의 빛에 대한 흡광성을 감안하여 HPLC-UVD를 사용하였다. 확립된 분석법에서 검량선의 상관계수($r^2$)는 0.99% 이상으로 우수한 직선성을 보였으며, 5개 대표 농산물에 imazapyr를 3개 농도에서 5회 반복하여 수행한 결과 회수율은 72.1-108.0%이었고 분석오차는 10% 미만으로 잔류농약 분석을 위한 CODEX 가이드라인(CAC/GL 40, 2003)에 적합하였다. 본 연구에서 확립된 분석법은 식품 중 imazapyr의 안전관리를 위한 공정분석법으로 사용될 것이다.

Keywords

References

  1. Beardmore, R. A., R. Hart, R. Iverson, M. A. Risely and M. Timmer (1991) Imazapyr herbicide. In: The imadazolinone Herbicides, CRC Press Inc. 211-227.
  2. Charles S. H. and A. D. Michael (1995) Improved Method for the analysis of imazapyr in soil. Pestic. Sci 4:21-26.
  3. Chemicalize by chemoxn ltd. (2014) (http://chemicalize.org).
  4. CAC (CODEX Alimentarius Commission) (2003) Guidelines on good laboratory practice in residue analysis, CAC/GL 40-1993, Rev.1-2003, Rome, Italy.
  5. CODEX (2012) http://www.codexalimentarius.org/download/report/777/REP12_PRe.pdf
  6. CODEX (2013) http://www.codexalimentarius.org/input/download/report/799/REP13_PRe.pdf
  7. CODEX (2014) http://www.codexalimentarius.org/input/download/report/917/REP14_PRe.pdf
  8. EFSA (European Food Safety Authority) (2014) http://www.efsa.europa.eu/fr/efsajournal/doc/3737.pdf
  9. MHLW (Ministry of Health, Labour and Walfare) (2014) http://www.sfs.fi/files/6914/GSPSNJPN380.pdf
  10. EPA (United states Environmental Protection Agency) (2003) https://www.federalregister.gov/articles/2003/09/26/03-24123/imazapyr-pesticide-tolerance
  11. EPA (United states Environmental Protection Agency) (2013) https://www.federalregister.gov/articles/2013/11/06/2013-26364/imazapyr-pesticide-tolerances
  12. EPA (United states Environmental Protection Agency) (2014) https://www.federalregister.gov/articles/2014/04/09/2014-07694/imazapyr-pesticide-tolerances
  13. Miller, J. H., R. J. Mitchell, and W. Deyou (1997) The manual of the forestry herbicide Science and technology press, Peking 98-107
  14. Navakova, O. (1997) Determination of imazethapyr and imazapyr residues in soil by coupled-column liquid chromatography. Chromatographia. 39(1/2):62-66
  15. Santoro, A., M. Mansour, M. Tropea, A. Scopa and S. A. Bufo (1999) Residual analysis of imazapyr and chlozolinate in water using sunlight, Bullletin of Environmental Contamination and Toxicology. Bull. Environ. Contam. Toxicol. 63:33-38. https://doi.org/10.1007/s001289900944
  16. Wang, X., H. Wang and D. Fan (2006) Degradation and metabolism of imazapyr in soils under aerobic and anaerobic conditions, international journal of environmental analytical chemistry. Intern. J. Environ, Anal. Chem. 86(8): 541-551. https://doi.org/10.1080/03067310500410730
  17. Weiping, L., P. Alba and G. Carlo (1992) High-performance liquid chromatographic determination of the herbicide imazapyr residues in water and soil. Sci. Total. Environ., 123/124:39-43. https://doi.org/10.1016/0048-9697(92)90130-K
  18. 식품의약품안전처 (2014) 식품공전.
  19. 이영득 (2013) 식품공전 잔류농약분석법 실무해설서, 식품의약품안전처.

Cited by

  1. A Study on Improvement of the Analytical Method of Chlorantraniliprole Residue in Herbal Medicine (Rehmannia glutinosa Libosch) using HPLC-UVD vol.25, pp.3, 2015, https://doi.org/10.7585/kjps.2021.25.3.196