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http://dx.doi.org/10.5338/KJEA.2018.37.1.05

Analytical Method for Flusulfamide as Benzenesulfonamide Fungicide, Residues in Major Agricultural Commodities  

Ahn, Kyung-Geun (Department of Herbal Medicine Resource, Kangwon National University)
Kim, Gi-Ppeum (Department of Herbal Medicine Resource, Kangwon National University)
Hwang, Young-Sun (Department of Biology, University of Texas-Arlington)
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.37, no.1, 2018 , pp. 57-65 More about this Journal
Abstract
BACKGROUND: An analytical method was developed using HPLC-UVD/MS to precisely determine the residue of flusulfamide, a benzenesulfonamide fungicide used to inhibit spore germination. METHODS AND RESULTS: Flusulfamide residue was 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 large volume of saline water and directly partitioned into dichloromethane 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. On an octadecylsilyl column in HPLC, flusulfamide was successfully separated from co-extractives of sample, and sensitively quantitated by ultraviolet absorption at 280 nm with no interference. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop sample fortified with flusulfamide at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries ranged from 82.3 to 98.2% 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 flusulfamide was 0.02 mg/kg as verified by the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique was also provided to clearly identify the suspected residue.
Keywords
Flusulfamide; HPLC-UVD/MS; Residue;
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