Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
권호 표지
DOI QR코드

DOI QR Code

Development of analytical method for Isotianil in agricultural commodities using GC-NPD and GC-MSD

GC-NPD와 GC-MSD를 이용한 농산물 중 Isotianil의 공정분석법 개발

  • Do, Jung-Ah (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Lee, Mi-Young (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Kang, Il-Hyun (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Kwon, Kisung (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration) ;
  • Oh, Jae-Ho (Food Chemical Residues Division, Department of Food Safety Evaluation, National Institute of Food and Drug Safety Evaluation, Food and Drug Administration)
  • 도정아 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 이미영 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 강일현 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 권기성 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과) ;
  • 오재호 (식품의약품안전청 식품의약품안전평가원 식품위해평가부 화학물질과)
  • Received : 2012.09.14
  • Accepted : 2012.10.15
  • Published : 2012.12.25
Download PDF
⟨ Previous Next ⟩

Abstract

Isotianil is a novel fungicide which induces systemic acquired resistance in plants. It has excellent preventive effects as low dosages against rice blast which is one of the most serious diseases in rice. The Maximum Residue Limit (MRL) of Isotianil in republic of korea was set to 0.1 mg/kg in rice, so it is necessary to determine levels of Isotianil residues in agricultural commodities for controlling food safety. Therefore, The purpose of this study was to develop analytical method for the determination of isotiical residues in agricultural commodities using GC-NPD/MSD. Isotianil was extracted with acetonitrile from apple, chinese cabbage, hulled rice, mandarin, pepper, and soybean. The extract was diluted with saline water, and then dichloromethane partition was followed to recover this fungcide from the aqueous phase. A solid phase extraction with Florisil cartridge was additionally employed for final clean up. Isotianil was analyzed and quantitated by GC-NPD and confirmed by GC-MSD. Average recovery of Isotianil ranged from 70.0 to 103.9% in six representative agricultural commodities with relative standard deviations less than 10%, and limit of quantification (LOQ) was 0.05 mg/kg.

Isotianil은 쌀 도열병을 방제하기 위한 새로이 개발된 식물활성 살균제로 다른 식물활성제에 비해 소량으로도 장시간의 효과를 나타내는 특징을 가지고 있다. 신규 농약 Isotianil에 대한 기준은 국내의 경우 2010년 쌀에 대하여 0.1 mg/kg으로 최초 설정되었으며, 이에 따른 식품 중 안전관리를 위해 Isotianil을 분석하기위한 검사법을 개발하였다. 검체 일정량에 acetonitrile을 가하고 균질화하여 대상농약을 추출하였으며, 액-액분배하고 florisil 카트리지를 이용한 고체상 추출 후 GC-NPD 및 GC-MSD로 분석하였다. 분석결과 농산물에 의한 간섭물질은 없었으며, 대표 농산물 현미 등 6 종에 대한 Isotianil의 분석 시험법의 정량한계와 직선성은 각각 0.05 mg/kg과 0.999($r^2$)이었다. 회수율은 대표 농산물에서 70.0~103.9%이었으며, 분석오차는 10% 미만으로 CODEX 잔류분석 기준에 적합하였다.

Keywords

References

  1. S. H. Ou, Rice disease. 2nd edition, Commonwealth Mycological Institute, Kew, Surrey, England., pp. 109- 200 (1985).
  2. 鄭鳳朝 외, 水稻의 病. 韓國植物保護 硏究 論考. pp1-31. 韓國植物保護學會 (1976).
  3. E. J. Lee, Panthogenic specialization of the rice blast fungus, Pyriculariorazae Cav (1978).
  4. O. Masaomi, Y. Tomoya, K. Atsushi and K. Orie, Applies development of a novel fungicide Isotianil. R&D report "SUMITOMO KAGAKU", 2011-1 (2011).
  5. H. Sawadasponsored by Jap. Plant port. Assoc, "New development of pest control measures by pesticide" Abstract (2008).
  6. H. W. Cheng, Y. G. Ha, M. H. Im, J. A. Do, J. H. Oh, Establishment of 22 pesticide MRLs in agricultural products based on risk assessment, Koren J. Env. Ari., 30(2), 166-172 (2011). https://doi.org/10.5338/KJEA.2011.30.2.166
  7. AOAC, Pesticide and industrial chemical residues, In official method of analysis, 17th.,pp1-88, AOAV International, Arlington, VA, USA (2000).
  8. US FDA, Pesticide Analytical Manual, Vol1: Multi residue Method (3rd ed), US Food and Drug Administration, USA (1999).
  9. Bayer to introduce two rice-pesticides in Japan : http://news.agropages.com
  10. New rice fungicide Isotianil granted regulatory approval in Japan:http://www.bayercropscience.com/bcsweb/cropprotection. nsf/id/EN_20100715/$file/2010-0366E.pdf
  11. C. H. Kown, M. I. Chang, M. H. Im, H. Choi, D. I. Jung and S. C. Lee, Anal. Sci. Tech., 1(6), 518-525 (2008).
  12. 이영득, 식품공전 잔류농약분석법 실무 해설서, 식품의약품안전평가원 (2012).