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Establishment of Analytical Method for Pymetrozine Residues in Crops Using Liquid-Liquid Extraction(LLE)

액-액 분배법을 활용한 작물 중 pymetrozine의 잔류분석법 확립

  • Yoon, Ji-Young (Department of Bio-Environmental Chemistry, Chungnam National University) ;
  • Moon, Hye-Ree (Department of Bio-Environmental Chemistry, Chungnam National University) ;
  • Park, Jae-Hun (Department of Bio-Environmental Chemistry, Chungnam National University) ;
  • Han, Ye-Hoon (Syngenta, Korea Ltd.) ;
  • Lee, Kyu-Seung (Department of Bio-Environmental Chemistry, Chungnam National University)
  • 윤지영 (충남대학교 농업생명과학대학 생물환경화학과) ;
  • 문혜리 (충남대학교 농업생명과학대학 생물환경화학과) ;
  • 박재훈 (충남대학교 농업생명과학대학 생물환경화학과) ;
  • 한예훈 (신젠타 코리아(주)) ;
  • 이규승 (충남대학교 농업생명과학대학 생물환경화학과)
  • Received : 2013.05.14
  • Accepted : 2013.06.19
  • Published : 2013.08.30

Abstract

Polar pesticides like pymetrozine (log $P_{ow}$: -0.18) are known to be difficult to analyze. The analytical method of pymetrozine using hydromatrix included in the official method of KFDA was uncommon and provided ambiguous evidence to confirm both the identity and the quantity. Therefore, precise single residue analytical method was developed in representative crops for using liquid-liquid extraction (LLE). The pymetrozine residue was extracted with methanol from 11 representative crops which comprised apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified serially by liquid-liquid extraction (LLE) and silica solid phase extraction (SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using $C_8$ column. LOQ (limit of quantitation) of pymetroizinie was 1 ng (S/N > 10) and MQL (method quantitation limit) was 0.01 mg/kg. Mean recoveries from 11 crop samples fortified at three levels (MQL, 10 ${\times}$ MQL and 50 ${\times}$ MQL) in triplicate were in the range of 83.1~98.5% with coefficients of variation (CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.

References

  1. Codex Alimentarius Commission (CAC) (2003) Guidelines on good laboratory practice in residue analysis, CAC/GL 40- 1993, Rev.1-2003, Rome, Italy.
  2. Cun, L., Y. Ting, H. Weiguo and W. Yinliang (2011) Residue and dynamics of pymetrozine in rice field ecosystem. Chemosphere. 82:901-904. https://doi.org/10.1016/j.chemosphere.2010.10.053
  3. Fuog, D., S.J. Fergusson and C. Fluckiger (1998) Pymetrozine: a novel insecticide affecting aphids and whiteflies, In: Ishaaya, I. and Degheele, D.(Eds), Insecticides with Novel Modes of Action: Mechanism and Application, Springer, Berlin, Germany, pp.40-49.
  4. Guoqing, S., H. Xuan and H. Yinan (2009) Kinetic study of the degradation of the insecticide pymetrozine in a vegetablefield ecosystem. J. Hazard. Mater. 164:497-501. https://doi.org/10.1016/j.jhazmat.2008.08.020
  5. Harrewijin, P. and H. Kayser (1997) Pymetrozine, a fast-acting and selective inhibitor of aphid feeding. In-situ studies with electronic monitoring of feeding behavior. Pestic. sci. 49:130-140. https://doi.org/10.1002/(SICI)1096-9063(199702)49:2<130::AID-PS509>3.0.CO;2-U
  6. Hong, J.H., C.R. Lee, J.S. Lim and K.S. Lee (2011) Comparison of analytical methods and residue patterns of pymetrozine in Aster scaber. Bull. Environ. Contam. Toxicol. 87:649-652. https://doi.org/10.1007/s00128-011-0407-8
  7. Hwang, J.I., Y.H. Jeon, H.Y. Kim, J.H. Kim, J.W. Ahn, D.R. Seok, Y.J. Lee, J.Y. Park, D.H. Kim and J.E. Kim (2011) Improvement of analytical method for rsidue pesticides in herbal medicines using macroporous diatomaceous earth column. Korean J. Environ. Agric. 5(2):140-148.
  8. Kayser, H., L. Kaufmann and F. Schurmann (1994) Pymetrozine (CGA 215, 944): a novel compound for aphid and whitefly control. An overview of its mode of action. Proc Brighton Crop protect conf-Pests and Diseases, BCPC, Alton, Hants, UK, pp.737-742.
  9. Korea Food & Drug Administration(KFDA) (2012) MRLs for Pesticide in Foods.
  10. Korea Food & Drug Administration(KFDA) (2012) Practical commentary Korean Food Standards Codex pesticide residues analysis method, third ed. pp. 1-91, 449-452.
  11. Kristinsson, H. (1994) Pymetrozine: A new insecticide, in: Briggs, G.G. (Eds), Advances in the Chemistry of insect Control III. The Royal Society of Chemistry, Cambridge, pp.85-102.
  12. Lee, H.R., M.J. Riu, E.H. Kim, J.K. Moon, J.A. Do, J.H. Oh, K.S. Kwon, M.H. Im, Y.D. Lee and J.H. Kim (2010) Establishment of analytical method for cyprodinil residue in apple, mandarin, Korean cabbage and green pepper. 2010. Korean J. Pestic. Sci. 14(4):371-380.
  13. Tomlin, C.D.S. (2009) The pesticide manual: A world compendium, fifteenth ed., BCPC, Hampshire, UK.
  14. Zhang, X., X. Cheng, C. Wang, Z. Xi and Q. Li (2007) Efficient high-performance liquid chromatography with liquid-liquid partition cleanup method for the determination of pymetrozine in tobacco. Annali di Chimica. 97:295-301. https://doi.org/10.1002/adic.200790015