Department of Herbal Medicine Resource, Kangwon National University1
Pesticide and Veterinary Drug Residues Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety2
Department of Horticultural Science, Kyungpook National University3
Division of Life and Environmental Science, Daegu University4
This experiment was conducted to establish an official determination method to measure fluazinam residue in horticultural crops for import and export using GC-ECD/MS. Fluazinam residue was extracted with acetone from fresh samples of four representative horticultural products, the vegetable crops green pepper and kimchi cabbage, and the fruit crops mandarin and apple. The acetone extract was diluted with saline water and n -hexane partitioning was used to recover fluazinam from the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fluazinam was separated and quantitated by GC with ECD using a DB-17 capillary column. The horticultural crops were fortified with three different concentrations of fluazinam. Mean recoveries ranged from 82.5% to 99.9% in the four crops. The coefficients of variation were less than 10.0%. The quantitative limit of fluazinam detection was 0.004 mgㆍkg-1 in the four crop samples. GC/MS with selected-ion monitoring was also used to confirm the suspected residue. This analytical method was reproducible and sensitive enough to measure the residue of fluazinam in horticultural commodities for import and export.
1. Ahn, K.G., G.H. Kim, G.P. Kim, Y.S. Hwang, S.B. Hong, Y.D. Lee, and M.G. Choung. 2015. Determination of quintozene residues in agricultural commodities using GC-ECD/MS. Korean J. Pestic. Sci. 19:195-203
2. AOAC. 2000. Pesticide and industrial chemical residues, In official method of analysis. 17th ed. Arlington, VA, USA. p. 88.
3. Codex Alimentarius Commission. 2003. Guidelines on good laboratory practice in residue analysis. CAC/GL 40-1993. Rev.1-2003. Rome. Italy.
4. Fong, W.G., H.A. Moye, J.N. Seiber, and J.P. Toth. 1999. Pesticide residues in food: methods, techniques, and regulations. John Wiley and Sons, NY, USA.
5. Guo, Z., H. Miyoshi, T. Komyoji, T. Haga, and T. Fujita. 1991. Uncoupling activity of a newly developed fungicide, fluazinam[3-chloro-N-(3-chloro-2,6-dinitro-4-trifluoromethylphenyl)-5-trifluoromethyl-2-pyridinamine]. Biochim. Biophys. Acta, Bioenerg. 1056:89-92.
6. Hu, W, S.J. Lee, and J.E. Kim. 1997. Adsorption-desorption, leaching, and degradation pattern of fungicide fluazinam in the soil environment. J. Korean Soc. Agric. Chem. Biotechnol. 40:128-133.
7. Jang, M.R., H.K. Moon, T.R. Kim, D.H. Yuk, J.H. Kim, and S.G. Park. 2010. Dietary risk assessment for pesticide residues of vegetable Seoul Korea. Korean J. Nutr. 43:404-412.
8. Kim, M.O., H.S. Hwang, M.S. Lim, J.E. Hong, S.S. Kim, J.A. Do, D.M. Choi, and D.H. Cho. 2010. Monitoring of residual pesticides in agricultural products by LC/MS/MS. Korean J. Food Sci. Technol. 42:664-675.
9. Kim, H.Y., S.H. Yoon, H.J. Park, H.J. Lee, I.S. Gwak, H.S. Moon, M.H Song, Y.M. Jang, M.S. Lee, J.S. Park, and K.H. Lee. 2007. Monitoring of residual pesticides in commercial agricultural products in Korea. Korean J. Food Sci. Technol. 39:237-245.
10. Korea Crop Protection Association. 2015. Using guideline of crop protection agents. Korea. p. 378.
11. Lee, J.H., H.W. Park, Y.S. Keum, C.H. Kwon, Y.D. Lee, and J.H. Kim. 2008. Dissipation pattern of boscalid in cucumber under greenhouse condition. Korean J. Pestic. Sci. 12:67-73.
12. Lee, S.J., Y.H. Kim, L.S. Song, and M.G. Choung. 2011. Determination of ametryn residue in agricultural commodities using HPLCUVD/ MS. Korean J. Pestic. Sci. 15:125-133.
13. Lee, S.J., Y.S. Hwang, Y.H. Kim, M.Y. Nam, S.B. Hong, W.K. Yun, C.H. Kwon, J.A. Do, M.H. Im, Y.D. Lee, and M.G. Choung. 2010. Determination of fomesafen residue in agricultural commodities using HPLC-UVD/MS. Korean J. Pestic. Sci. 14:95-103.
14. Lee, Y.D. 2012. Pesticide Analytical Residues Manual in Food Code. MFDS.
15. Miller, J.M. 2005. Chromatography : Concepts and Contrasts. 2nd ed. Wiley Interscience, USA. p. 286.
16. Ministry of Food and Drug Safety 2012. Korea Food Code. Korea. p. 10-4-340.
17. Ministry of Food and Drug Safety 2012. Korea Food Code. Korea. p. 10-4-9.
18. Ministry of Food and Drug Safety 2014. MRLs for Pesticides in Foods. Korea. p. 100. Krieger, R. 2001. Handbook of pesticide toxicology, Vol.2 Set: principles and agents. Academic press, USA. p. 1243.
19. Ulrich, S., J. Peter, and W. Matthias. 2012. Modern crop protection compounds: herbicides. John Wiley & Sons, Germany. p. 662.
20. United States Environmental Protection Agency. 2001. Pesticide fact sheet for fluazinam. Washington D.C., USA.