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http://dx.doi.org/10.5338/KJEA.2015.34.4.50

Development of Analytical Method for Fipronil Residues in Agricultural Commodities Using GC-ECD/MS  

Ahn, Kyung-Geun (Department of Herbal Medicine Resource, Kangwon National University)
Kim, Gyeong-Ha (Department of Herbal Medicine Resource, Kangwon National University)
Kim, Gi-Ppeum (Department of Herbal Medicine Resource, Kangwon National University)
Hwang, Young-Sun (Department of Herbal Medicine Resource, Kangwon National University)
Kang, In-Kyu (Department of Horticultural Science, Kyungpook National University)
Lee, Young Deuk (Division of Life and Environmental Science, Daegu University)
Choung, Myoung-Gun (Department of Herbal Medicine Resource, Kangwon National University)
Publication Information
Korean Journal of Environmental Agriculture / v.34, no.4, 2015 , pp. 309-317 More about this Journal
Abstract
BACKGROUND: An analytical method was developed using GC-ECD/MS to precisely determine the residue of fipronil, a phenylpyrazole insecticide used to control a wide range of foliar and soil-borne pests.METHOD AND RESULTS: Fipronil residue was extracted with acetone from representative samples of five raw products which comprised hulled rice, soybean, Kimchi cabbage, green pepper, and apple. The extract was diluted with saline water, and fipronil was partitioned into n-hexane/dichloromethane (20/80, v/v) to remove polar co-extractives in the aqueous phase. Florisil column chromatography was additionally employed for final purification of the extract. Fipronil was separated and quantitated by GC-ECD using a DB-17 capillary column. Accuracy of the proposed method was validated by the recovery from crop samples fortified with fipronil at 3 levels per crop in each triplication.CONCLUSION: Mean recoveries ranged from 86.6% to 106.0% in five representative agricultural commodities. The coefficients of variation were less than 10%. Limit of quantitation of fipronil was 0.004 mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of fipronil in agricultural commodities.
Keywords
Fipronil; GC-ECD/MS; Residue;
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Times Cited By KSCI : 1  (Citation Analysis)
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1 Lee, J. H., Park, H. W., Keum, Y. S., Kwon, C. H., Lee, Y. D., & Kim, J. H. (2008). Dissipation pattern of boscalid in cucumber under greenhouse condition. The Korean Journal of Pesticide Science, 12(1), 67-73.
2 Kwon, C. H., & Lee, Y. D. (2003). Terminal residues of monocrotophos and phosphamidon in apples. Life Science Research, 1(3), 277-286.
3 Korea Crop Protection Association, (2015). Using guideline of crop protection agents, p. 735. Korea Crop Protection Association, Korea.
4 Hadjmohammadi, M. R., Nikou, S. M., & Kamel, K. (2006). Determination of fipronil residue in soil and water in the rice fields in north of Iran by RP-HPLC method. Acta Chimica Slovenica, 53(4), 517-520.
5 Fong, W. G., Moye, H. A., Seiber, J. N., & Toth, J. P. (1999). Pesticide residues in food: Methods, technologies, and regulations. pp. 3-4, 40-44, Canada.
6 Codex Alimentarius Commission. (2003). Guidelines on good laboratory practice in residue analysis. CAC/GL 40-1993, Rev.1-2003, Rome, Italy.
7 Cella, A. L., Moura-Andrade, G. C. R., Freguglia, R. M. O., & Tornisielo, V. L. (2012). Evaluation of organochlorine pesticide residues and fipronil in Corumbataí river basin, Piracicaba, São Paulo, Brazil. Journal of pharmacy, 2(5), 61-66.
8 Vılchez, J. L., Prieto, A., Araujo, L., & Navalon, A. (2001). Determination of fipronil by solid-phase microextraction and gas chromatography–mass spectrometry. Journal of Chromatography A, 919(1), 215-221.   DOI
9 Tomlin, C. D. S. (2006). The pesticide manual: a world compendium. 14th ed. pp.462-464, Hampshire, England.
10 Ock, H. S. (2009). Developmental trend of analytical methods for pesticide residues. The Korean Journal of Pesticide Science, 13(4), 336-348.
11 Miller, J. M. (2005). Chromatography: concepts and contrasts. 2nd ed. pp. 286-287, John Wiley & Sons, USA.
12 Lee, S. J., Kim, Y. H., Song, L. S., Hwang, Y. S., Lim, J. D., Sohn, E. H., Im, M. H., Do, J. A., Oh, J. H., Kwon, K. S., Lee, J. K., Lee, Y. D., & Choung, M. G. (2011). Development of analytical method for Fenoxycarb, Pyriproxyfen and Methoprene residues in agricultural commodities using HPLC-UVD/MS. The Korean Journal of Pesticide Science, 15(3), 254-268.
13 Lee, S. J., Kim, Y. H., Song, L. S., & Choung, M. G. (2011). Determination of Ametryn Residue in Agricultural Commodities Using HPLC-UVD/MS. The Korean Journal of Pesticide Science, 15(2), 125-133.
14 Lee, S. J., Kim, Y. H., Hwang, Y. S., Kwon, C. H., Do, J. A., Im, M. H., Lee, Y. D., & Choung, M. G. (2010). Determination of methoxyfenozide, chromafenozide and tebufenozide residues in agricultural commodities using HPLC-UVD/MS. The Korean Journal of Pesticide Science, 14(1), 37-48.
15 Lee, S. J., Hwang, Y. S., Kim, Y. H., Kwon, C. H., Do, J. A., Im, M. H., Lee, Y. D., & Choung, M. G. (2010). Determination of Captan, Folpet, Captafol and Chlorothalonil Residues in Agricultural Commodities using GC-ECD/MS. Korean Journal of Environmental Agriculture, 29(2), 165-175.   DOI