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HPLC-UVD/MS를 이용한 농산물 중 Cyromazine의 잔류분석법
송이슬(Lee-Seul Song),김영학(Young-Hak Kim),이수진(Su-Jin Lee),황영선(Young-Sun Hwang),권찬혁(Chan Hyeok Kwon),도정아(Jung-Ah Do),오재호(Jae-Ho Oh),임무혁(Moo Hyeog Im),장우석(Woo-Suk Chang),이영득(Young Deuk Lee),정명근(Myoung-Gun C 한국농약과학회 2012 농약과학회지 Vol.16 No.3
A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq C18 column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.
수도 재배환경 중 제초제 Cyclosulfamuron 의 잔류특성
이영득(Young Deuk Lee),송성도(Sung Do Song) 한국환경농학회 2001 한국환경농학회지 Vol.20 No.4
Several experiments including persistence, distribution, leaching, and terminal residue trials were carried out to investigate the behavior of cyclosulfamuron in rice paddies. Cyclosulfamuron was gradually dissipated in two different soils showing the first-order kinetics. Half-lives of the herbicide were calculated to be 17∼30 and 14∼16 days under field and laboratory conditions, respectively. In the paddy soil/water system, the residue tended to reside more in the soil phase as time elapsed. Cyclosulfamuron was less persistent in paddy water than in soil with half-lives of 10 and 19 days, respectively. No cyclosulfamuron was leached below 20 ㎝-deep soil during water percolation with 50 cm hydraulic head, while some downward mobility was observed within the soil column. When EC and SC formulations of cyclosulfamuron were applied to the paddy field at 120 or 150-day pre-harvest intervals, its terminal residues in hulled rice were all less than 0.01 ㎎/㎏, irrespective of formulation type and application timing. In rice straw, however, some residues were found at <0.02∼0.05 ㎎/㎏ as SC formulation was applied. Rapid dissipation, restricted mobility, and low terminal residues of cyclosulfamuron in rice paddies suggest that no significant residues would be transported or carried over to the non-target environment.
HPLC-UVD/MS를 이용한 농산물 중 bentazone의 분석법 확립
김영학(Young-Hak Kim),이수진(Su-Jin Lee),송이슬(Lee-Seul Song),황영선(Young-Sun Hwang),이영득(Young Deuk Lee),정명근(Myoung-Gun Choung) 한국농약과학회 2011 농약과학회지 Vol.15 No.2
Bentazone is benzothiadiazole group herbicide, and used to foliage treatment. This herbicide have already been widely used for cereals and vegetables planting in worldwide. This experiment was conducted to establish a determination method for bentazone residue in crops using HPLC-UVD/MS. Bentazone residue was extracted with acetone (adjusted pH 1 with phosphoric acid) from representative samples of five raw products which comprised hulled rice, soybean, apple, green pepper, and Chinese cabbage. The extract was diluted with saline water, and dichloromethane partition was followed to recover bentazone from the aqueous phase. Florisil column chromatography was additionally employed for final clean up of the extract. The bentazone was quantitated by HPLC with UVD, using a YMC ODS AM 303 (4.6 × 250 ㎜) column. The crops were fortified with bentazone at 3 levels per crop. Mean recovery ratio were ranged from 82.0% for a 0.2 ㎎/㎏ in apple to 97.9% for a 0.02 ㎎/㎏ in Chinese cabbage. The coefficients of variation were ranged from 0.5% for a 0.02 ㎎/㎏ in soybean to 9.7% for a 0.02 ㎎/㎏ in Chinese cabbage. Quantitative limit of bentazone was 0.02 ㎎/㎏ in representative five crop samples. A LC/MS with selected-ion monitoring was also provided to confirm the suspected residue. Therefore, this analytical method was reproducible and sensitive enough to determine the residue of bentazone ill agricultural commodities.