Monitoring of Neonicotinoid Pesticide Residues in Paprika Using UPLC-MS/MS from Gyeongnam Region

UPLC-MS/MS를 이용한 경남지역 파프리카 중 neonicotinoid계 농약 잔류 모니터링

  • Kim, Nam-Kuk (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Lee, Seung-Hwa (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Nam, Yu-Jeong (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Moon, Kyung-Mi (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Park, Min-Ho (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Yun, Mun-Hee (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Kim, Mi-Young (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Jang, Hyun-Min (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS)) ;
  • Shin, Bong-Shig (Gyeongnam Provincial Office, National Agricultural Products Quality Management Service (NAQS))
  • 김남국 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 이승화 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 남유정 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 문경미 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 박민호 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 윤문희 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 김미영 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 장현민 (국립농산물품질관리원 경남지원 조사분석과) ;
  • 신봉식 (국립농산물품질관리원 경남지원 조사분석과)
  • Received : 2011.01.18
  • Accepted : 2011.02.03
  • Published : 2011.03.31

Abstract

Monitoring or follow-up surveying pesticide residues in agricultural commodities is the key to meet the international regulations and to enhance international competitiveness of Korean agricultural commodities. Six neonicotinoid insecticides, acctamiprid, clothianidin, dinotefuran, imidacloprid, thiacloprid, and thiamethoxam were monitored in 95 paprika samples collected from Gyeongnam area. Thc pesticide residues were extracted by EN 15662 buffer based on the QuEChERS method, clean-upped with dispersive solid-phase extraction method to remove interfering pigments, and analyzed using UPLC-MS/MS. The neonicotinoid pesticides were detected in 90.5% of the paprika samples. Two or more pesticides were detected in 82.3% of samples. Although detection frequencies were high, all samples complied with the maximum residue limits (MRLs) set by both the Korea Food and Drug Administration (KFDA) and Japanese Ministry of Health, Labour and Welfare.

본 연구는 QuEChERS 방법에 기초한 EN15662 buffer 및 dSPE, UPLC-MS/MS플 활용하여 경남지역에서 생산되는 대일 수출용 파프리카 내 neonicotinoid계 농약성분의 잔류성 실태 조사를 위하여 수행하였다. 6종의 neonicotinoid계 농약의 회수율 및 변이계수는 0.05 및 0.5 mg/kg 수준에서 각각 84.0~92.7(${\pm}0.0{\sim}3.8%$)과 95.1~98.9%(${\pm}0.9{\sim}5.2%$)로 나타났다. 분석에 사용된 95시료 중 90.3%에서 농약성분이 검출되었으며, 82.3%에서 2종이상의 농약성분이 검출되었다. 검출된 농약의 농도는 0.01~1.63 mg/kg으로 나타났고, 농약성분 중 dinotefuran 및 imidacloprid가 78.1 및 65.6%의 빈도를 보였다. 6종의 농약 중 thiacloprid가 8.3%로 분석된 농약 중 가장 낮은 빈도를 나타내었다. 그러나 검출된 농약의 경우 모두 한국 및 일본의 잔류허용기준을 초과하지 않는 것으로 나타나, 경남지역 생산 대일 수출용 파프리카의 경우 neonicotinoid 계 농약에 대한 사용이 안전한 수준으로 잘 관리되고 있음을 확인하였다.

Keywords

References

  1. Bai, D., Lummis, S., Leicht, W., Breer, H., Sattelle, D. (1991) Actions of imidacloprid and a related nitromethylene on cholinergic receptors of an identified insect motor neurone. Pesticide science 33(2):197-204. https://doi.org/10.1002/ps.2780330208
  2. Di Muccio, A., Fidente, P., Barbini, D., Dommarco, R., Seccia, S., Morrica, P. (2006) Application of solid-phase extraction and liquid chromatography-mass spectrometry to the deter-mination of neonicotinoid pesticide residues in fruit and vegetables. Journal of Chromatography A 1108(1):1-6. https://doi.org/10.1016/j.chroma.2005.12.111
  3. FAD (1999) Pesticide analytical manual. Vol. I. Section 103: Method application in regulatory analysis (103-1).
  4. Jenke, D. (1996) Chromatographic Method Validation: A Review of Current Practices and Procedures. II. Guidelines for Primary Validation Parameters. Journal of Liquid Chromatography & Related Technologies 19(5):737-757. https://doi.org/10.1080/10826079608005534
  5. Lehotay, S. J. (2007) Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate: collaborative study. Journal of AOAC International 90(2):485-520.
  6. Liu, S., Zheng, Z., Wei, F., Ren, Y., Gui, W., Wu, H., Zhu, G. (2010) Simultaneous Determination of Seven Neonicotinoid Pesticide Residues in Food by Ultraperformance Liquid Chromatography Tandem Mass Spectrometry. Journal of Agricultural and Food Chemistry 58(6):3271-3278. https://doi.org/10.1021/jf904045j
  7. MacDougall, D., Crummett, W. (1980) Guidelines for data acquisition and data quality evaluation in environmental chemistry. Analytical Chemistry 52(14): 2242-2249. https://doi.org/10.1021/ac50064a004
  8. Matsuda, K., Buckingham, S., Kleier, D., Rauh, J., Grauso, M., Sattelle, D. (2001) Neonicotinoids: insecticides acting on insect nicotinic acetylcholine receptors. Trends in pharmaco-logical sciences 22(11):573-580. https://doi.org/10.1016/S0165-6147(00)01820-4
  9. Mills, P.A., Onley, J.H. Gaither, R.A. (1963) Rapid method for chlorinated pesticide residues in non-fatty foods. Journal of the Association of Official Agricultural Chemists 46:186-191.
  10. Nauen, R., Bretschneider, T. (2002) New modes of action of insecticides. Pesticide Outlook 13(6):241-245. https://doi.org/10.1039/b211171n
  11. Obana, H., Okihashi, M., Akutsu, K., Kitagawa, Y., Hori, S. (2003) Determination of neonicotinoid pesticide residues in vegetables and fruits with solid phase extraction and liquid chromatography mass spectrometry. Journal of Agricultural and Food Chemistry 51(9):2501-2505. https://doi.org/10.1021/jf0261102
  12. Philip, W. L. (2003) Handbook of residue analytical methods for agrochemicals. I, p. 13-17.
  13. Swartz, M. (2005) UPLC$^{TM}$: an introduction and review. Journal of Liquid Chromatography & Related Technologies 28(7): 1253-1263. https://doi.org/10.1081/JLC-200053046
  14. Zhang, A., Kaiser, H., Maienfisch, P., Casida, J. (2000) Insect nicotinic acetylcholine receptor: conserved neonicotinoid specificity of [3H] imidacloprid binding site. Journal of neurochemistry 75(3):1294-1303.
  15. 농수산물유통공사 (2010) 농수산물무역정보: 2009년 농림수산식품수출실적.
  16. 농촌진흥청 (2010) 농약관리법령 고시 예규집. pp. 242-246.
  17. 옥환석 (2009) 잔류농약 분석방법의 개발 동향. 농약과학회지 13(4):336-348.
  18. 이영득, 김찬섭, 임양빈, 오병렬, 이병무, 박병준, 최주현 (2004) Neonicotinoid계 농약의 잔류분석법 개발. 농업과학기술원 pp.141-163.