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http://dx.doi.org/10.5338/KJEA.2018.37.2.12

Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS  

Ahn, Kyung Geun (Department of Herbal Medicine Resource, College of Health Science, Kangwon National University)
Kim, Gi Ppeum (Department of Herbal Medicine Resource, College of Health Science, Kangwon National University)
Hwang, Young Sun (Department of Biology, University of Texas-Arlington)
Kang, In Kyu (Department of Horticultural Science, College of Agriculture and Life Sciences, Kyungpook National University)
Lee, Young Deuk (Division of Life and Environmental Science, College of Science Life Integration, Daegu University)
Choung, Myoung Gun (Department of Herbal Medicine Resource, College of Health Science, Kangwon National University)
Publication Information
Korean Journal of Environmental Agriculture / v.37, no.2, 2018 , pp. 104-116 More about this Journal
Abstract
BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) 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 residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.
Keywords
Chloroacetamide; Dinitroaniline; Diphenyl ether; GC-ECD/MS; Residues;
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Times Cited By KSCI : 1  (Citation Analysis)
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1 Li, H. P., Li, G. C., & Jen, J. F. (2004). Fast multi-residue screening for 84 pesticides in tea by gas chromatography with dual-tower auto-sampler, dualcolumn and dual detectors. Journal of the Chinese Chemical Society, 51(3), 531-542.   DOI
2 Mastovska, K., Dorweiler, K. J., Lehotay, S. J., Wegscheid, J. S., & Szpylka, K. A. (2010). Pesticide multiresidue analysis in cereal grains using modified QuEChERS method combined with automated direct sample introduction GC-TOFMS and UPLC-MS/MS techniques. Journal of Agricultural and Food Chemistry, 58(10), 5959-5972.   DOI
3 Miller, J. M. (2005). Chromatography : Concepts and contrasts, standardization administration of the people's republic. pp. 286-287. (2nd), Wiley Intersciense, USA.
4 Park, C. J., & Lee, Y. D. (2003). Persistence of the fungicide boscalid in grapes and strawberries, Life Science Research, 2(2), 9-16.
5 Ahn, K. G., Kim, G. H., Kim, G. P., Kim, M. J., Hwang, Y. S., Hong, S. B., Lee, Y. D., & Choung, M. G. (2014). Determination of amisulbrom residues in agricultural commodities using HPLC-UVD/MS. Korean Journal of Pesticide Science, 18(4), 321-329.   DOI
6 Canadian Council of Ministers of the Environment (1999). Canadian water quality guidelines for the protection of aquatic life, metolachlor, pp. 1-3. Manitoba Statutory Publications, Canada.
7 Dharumarajan, S., Sankar, R., Baskar, A., & Kumar, K. (2008). Persistence of pretilachlor in coastal rice ecosystem. Pesticide Research Journal, 20(2), 273-274.
8 Fong, W. G., Moye, H. A., Seiber, J. N., & Toth, J. P. (1999). Pesticide residues in food: methods. Technologies, and Regulations, pp. 3-44, Wiley Interscience, Canada.
9 Hutson, D. H. (1998). Metabolic pathways of agrochemicals, herbicides and plant growth regulators. pp. 216-217. Cambridge, UK.
10 Raina, R., & Hall, P. (2008). Comparison of gas chromatography -mass spectrometry and gas chromatography-tandem mass spectrometry with electron ionization and negative-ion chemical ionization for analyses of pesticides at trace levels in atmospheric samples. Analytical chemistry insights, 3, 111-125.
11 Judge, C. A., Neal, J. C., & Leidy, R. B. (2003). Trifluralin (Preen) dissipation from the surface layer of a soilless plant growth substrate. Journal of Environmental Horticulture, 21(4), 216-222.
12 Jursik, M., Andr, J., Holec, J., & Soukup, J. (2011). Efficacy and selectivity of post-emergent application of flumioxazin and oxyfluorfen in sunflower. Plant Soil Environment, 57(11), 532-539.   DOI
13 Kim, M. O., Hwang, H. S., Lim, M. S., Hong, J. E., Kim, S. S., Do, J. A., Choi, D. M., & Cho, D. H. (2010). Monitoring of residual pesticides in agricultural products by LC/MS/MS. Korean Journal of Food Science and Technology, 42(6), 664-675.
14 Kwon, C. H., & Lee, Y. D. (2003). Terminal residues of monocrotophos and phosphamidon in apples. Life Science Research, 1(3), 277-286.
15 Yun, H. C., Park, J. H., Cha, K. S., Youn, J. B., Jeong, J. H., Park, J. Y., Lee, J. Y., Kim, J. M., & Kang, J. M. (2009). Monitoring the residual pesticide levels of soil and water from the main agricultural area in Busan (II). The Annual Report of Busan Metropolitan City Institute of Heath & Environment, 19(1), 72-80.
16 Shackelford, D. D., McCormick, R. W., West, S. D., & Turner, L. G. (2000). Determination of ethalfluralin in canola seed, meal, and refined oil by capillary gas chromatography with mass selective detection. Journal of agricultural and food chemistry, 48(9), 4422-4427.   DOI
17 The Dow Chemical Company (2010). Product safety assessment for ethalfluralin. pp. 1-6. www.dow.com/productsafety/finder/.
18 Yokley, R. A., Mayer, L. C., Huang, S. B., & Vargo, J. D. (2002). Analytical method for the determination of metolachlor, acetochlor, alachlor, dimethenamid, and their corresponding ethanesulfonic and oxanillic acid degradates in water using SPE and LC/ESI-MS/MS. Analytical chemistry, 74(15), 3754-3759.   DOI
19 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. Korean Journal of Pesticide Science, 12(1), 67-73.
20 Barefoot, A., Murphy, J., & Aizawa, H. (2003). Handbook of residue analytical methods for agrochemicals (Vol. 2). Lee, P. W. (ed.). p. 585, Chichester, West Sussex, England; Hoboken, NJ: Wiley.
21 Lee, S. J., Kim, Y. H., Song, L. S., & Choung, M. G. (2011). Determination of ametryn residue in agricultural commodities using HPLC-UVD/MS. Korean Journal of Pesticide Science, 15(2), 125-133.
22 Lerch, R. N., Ferrer, I., Thurman, E. M., & Zablotowicz, R. M. (2003). Identification of trifluralin metabolites in soil using ion-trap LC/MS/MS, American Chemical Society, 291-310. DOI: 10.1021/bk-2003-0850.ch017