HPLC-UVD/MS를 이용한 농산물 중 Amisulbrom의 잔류분석

Abstract

Abstract This experiment was conducted to establish an analytical method for residues of amisulbrom, asrecently developed an oomycete-specific fungicide showing inhibition of fungal respiration, in crops usingHPLC-UVD/MS. Amisulbrom residue was extracted with acetonitrile from representative samples of five rawproducts which comprised apple, green pepper, kimchi cabbage, potato and hulled rice. The extract was dilutedwith 50 mL of saline water and directly partitioned into dichloromethane to remove polar co-extractives in theaqueous phase. For the hulled rice sample, n-hexane/acetonitrile partition was additionally employed to removenon-polar lipids. The extract was finally purified by optimized Florisil column chromatography. On anoctadecylsilyl column in HPLC, amisulbrom was successfully separated from sample co-extractives andsensitively quantitated by ultraviolet absorption at 255 nm with no interference. Accuracy and precision of theproposed method was validated by the recovery test on every crop samples fortified with amisulbrom at 3concentration levels per crop in each triplication. Mean recoveries ranged from 85.3% to 105.6% in fiverepresentative agricultural commodities. The coefficients of variation were all less than 10%, irrespective ofsample types and fortification levels. Limit of quantitation (LOQ) of amisulbrom was 0.04 mg/kg as verifiedby the recovery experiment. A confirmatory method using LC/MS with selected-ion monitoring technique wasalso provided to clearly identify the suspected residue. The proposed method was sensitive, reproducible andeasy-to-operate enough to routinely determine the residue of amisulbrom in agricultural commodities.Key words Amisulbrom, HPLC-UVD/MS, Residue