DOI QR코드

DOI QR Code

Development and validation of analytical methods for pyrifluquinazon residues determination on agricultural commodities by HPLC-UVD

HPLC-UVD를 이용한 농산물 중 pyrifluquinazon 잔류시험법 개발 및 검증

  • Do, Jung-Ah (Pesticide & Veterinary Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Kwon, Ji-Eun (Pesticide & Veterinary Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Kim, Mi-Ra (Daejeon Regional FDA) ;
  • Lee, Eun-Mi (Daejeon Regional FDA) ;
  • Kuk, Ju-Hee (Gwangju Reginal FDA) ;
  • Cho, Yoon-Jae (Pesticide & Veterinary Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Chang, Moon-Ik (Pesticide & Veterinary Residues Division, National Institute of Food and Drug Safety Evaluation) ;
  • Kwon, Kisung (Busan Reginal FDA) ;
  • Oh, Jae-Ho (Pesticide & Veterinary Residues Division, National Institute of Food and Drug Safety Evaluation)
  • 도정아 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 권지은 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 김미라 (대전지방식품의약품안전청 유해물질분석팀) ;
  • 이은미 (대전지방식품의약품안전청 유해물질분석팀) ;
  • 국주희 (광주지방식품의약품안전청 유해물질분석팀) ;
  • 조윤제 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 장문익 (식품의약품안전처 식품의약품안전평가원 잔류물질과) ;
  • 권기성 (부산지방식품의약품안전청 시험분석센터) ;
  • 오재호 (식품의약품안전처 식품의약품안전평가원 잔류물질과)
  • Received : 2013.02.27
  • Accepted : 2013.06.12
  • Published : 2013.06.25

Abstract

Pyrifluquinazon is classified with a quinazoline insecticide that regulates food intake by controling the feeding behavior acting on the endocrine or nervous system of pests such as aphids and white fly. To keep safety on pyrifluquinazon residues in agricultural commodities a simple, accurate and rapid analytical method was developed and validated using high performance liquid chromatograph (HPLC-UVD). The pyrifluquinazon residues acidified with 1% formic acid in samples were extracted with acetonitrile and partitioned with hexane subsequently to dichloromethane then purified with silica solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-UVD. The method was validated using apple and pear spiked with pyrifluquinazon at 0.02, 0.05 and 0.1 mg/kg and hulled rice, pepper, soybean at 0.05 and 0.1 mg/kg. Average recoveries were 70.5~107.9% with relative standard deviation less than 10%. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional FDA and Daejeon regional FDA was followed with Codex guideline (CODEX CAC/GL 40). This method is appropriated at pyrifluquinazon residues determination and will be used as official method of analysis.

Pyrifluquinazon은 quinazoline 계통의 살충제로 진딧물, 흰파리 등 해충에 대해 음식섭취를 조절하는 신경계 또는 내분비계에 작용하여 섭식행동을 제어하고 또한 식물조직에 추가적 손상을 방지, 식물체 바이러스 확산을 막는 역할을 한다. 국내에는 2012년 사과와 배에 신규 사용등록되어 식품의약품안전처에서 잔류허용기준을 설정하였다. 본 농약은 분자량이 464.3으로 큰 편이며, 증기압이 낮아 분석을 위한 기기로 HPLC-UVD를 선택하여 잔류허용기준 준수여부 확인을 위한 시헙법을 확립하였다. 추출용매는 간섭물질의 추출이 비교적 적은 acetonitrile을 사용하였으며, pyrifluquinazon의 Log $P_{ow}$값이 3.12로 극성에 가까운 물리화학적 특성을 감안하여 액-액 분배를 위한 용매로 dichloromethane을 사용하였다. 간섭물질 제거를 위한 clean-up과정에서는 silica 카트리지를 사용하였고, acetone으로 용출하여 최적의 정제조건을 확립하였다. 분석 결과 회수율은 70~120%로 나타났으며, 분석오차는 10% 미만, 실험실간 편차 ($RSD_R$(%)) > 0.01 mg/kg, ${\leq}$0.1 mg/kg 범위에서 3.40~15.4%로 코덱스 가이드라인 기준에 적합함을 확인 하였다. 또한 본 시험법의 재현성 및 선택성을 추가로 확보할 수 있도록 LC-MS를 통한 정성시험법을 추가로 확립하였다. 본 시험법은 신규 등록된 pyrifluquinazon 분석을 위한 신속 정확한 공정 시험법으로 식품공전에 등재되어 활용되고 있다.

Keywords

References

  1. A. K. Min, Insecticidal activity and feeding behavior of green peach Aphid, Myzus persicae against Nano type of Pyrifluquinazon, Master Thesis, Chungnam National University (2011).
  2. 農評書, ピリフルキナゾン, Food Safety Commission (2009).
  3. Andy Beer: Agrow US EPA to OK Nichino's Pyrifluquinazon (2012) available at http://www.agrow.com/ newproducts/US-EPA-to-OK-Nichinos-pyrifluquinazon.
  4. Palmer C and Vea E.: IR-4 Ornamental Horticulture Program, Pyrifluquinazon, Crop Safety and Efficacy (2010).
  5. The Japan Food Chemical Research Foundation, avaliable at http://www.m5.ws001.squarestart.ne.jp/foundation/ search.html
  6. 국립농업과학원, 농산물 중 농약잔류분 정의 및 분석방법 정리, avaliable at http://www.naas.go.kr/_ Include/down.asp?idx=8608&fileMode=0&dnGubun =1&tg=1
  7. GUIDANCE DOCUMENT ON THE DEFINITION OF RESIDUE, OECD Residue Chemistry Export Group.
  8. Pyrifluquinazon WG의 작물(사과) 잔류성 시험 보고서 요약본, (주) 경농(2008).
  9. 이영득: 식품공전 잔류농약 분석법 실무해설서 (2012)
  10. Codex Alimentarius Commission, Guidelines on good laboratory practice in residue analysis. CAC/GL 40-1993. Rome. Italy (2003).
  11. S. J. Lee, Y. H. Kim, L. W. Song, Y. S. Hwang, J. D. Lim, E. H. Sohn, M. H. Im, J. A. Do, J. H. Oh, K. S. Kwon, J. K. Lee, Y. D. Lee and M. G. Choung: Development of analytical method for Fenoxycarb, Pyriproxyfen and Methoprene residues in agricultural commodities using HPLC-UVD/MS, Korean Journal of Pesticide Science, 15(3), 254-268 (2011).
  12. C. H. Kwon, M. H. Chang, M. H. Im, D. I. Choi, S. C. Jung, J. Y. Lee, Y. D. Yu, J. O. Lee and M. K. Hong: Determination of mandipropamid residues in agricultural commodities using high-performance liquid chromatography with mass spectrometry, Anal. Sci. Technol, 21(6), 518-525 (2008).

Cited by

  1. Simultaneous determination of pyrifluquinazon and its main metabolite in fruits and vegetables by using QuEChERS-HPLC-MS/MS vol.40, pp.3, 2017, https://doi.org/10.1002/jssc.201601094