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Determination of Cyhalofop-butyl and its Metabolite in Water and Soil by Liquid Chromatography
헴리나,최정희,유학,카이사티아,심재한,Hem, Lina,Choi, Jeong-Heui,Liu, Xue,Khay, Sathya,Shim, Jae-Han The Korean Society of Pesticide Science 2008 농약과학회지 Vol.12 No.4
실험실 내 조건에서, 물과 토양 중 cyhalofop-butyl과 그 대사물질인 cyhalofop acid를 위한 잔류분석법이 고감도에서도 간단하고 매우 효과적으로 개발되었다. 물과 토양 중 cyhalofop-butyl과 cyhalofop acid를 분석하기 위하여 액액분별추출과 silica gel chromatographic 정제를 수행하였으며 HPLC-UV를 이용하여 정성/정량하였다. cyhalofop-butyl의 회수율은 2 가지 농도에서 3 반복 수행하여 각각 82.5-100.0%와 66.7-97.9%이었고, 검출한계와 최소검출량은 두 시료에서 모두 0.02 ppm과 10 ng이었다. Cyhalofop acid의 회수율은 물과 토양에서 각각 80.7-104.8%와 76.9-98.1%이 었으며, 검출한계는 각각 0.005 ppm과 0.01 ppm이었고 최소검출량은 두 시료에서 모두 2 ng이었다. Cyhalofop-butyl의 반감기는 물과 토양에서 각각 4.14와 6.6 day였다. 개발되어진 본 시험법은 cyhalofop-butyl의 30% 유탁제를 처리한 물과 토양에서 그 잔류량을 분석하기 위하여 성공적으로 적용되었다. In this study, a simple, effective, and sensitive method has been developed for the quantitative residue analysis of cyhalofop-butyl and its metabolite cyhalofop acid in water and soil when kept under laboratory conditions. The content of cyholofop-butyl and cyhalofop acid in water and soil was analyzed by first purifying the compounds through liquid-liquid extraction and partitioning followed by Silica gel (adsorption) chromatography. Upon the completion of the purification step the residual levels were monitored through high-performance liquid chromatography (HPLC) using a UV absorbance detector. The recoveries of cyhalofop-butyl from three replicates spiked at two different concentrations ranged from 82.5 to 100.0% and from 66.7 to 97.9% in water and soil, respectively. The limit of detection and minimum detection level of cyhalofop-butyl in water and soil was 0.02 ppm and 10 ng, respectively. The recoveries of cyhalofop acid ranged from 80.7 to 104.8% in water and from 76.9 to 98.1 % in soil. The limit of detection of cyhalofop acid was 0.005 ppm in water and 0.01 ppm in soil, while the minimum detection level was 2 ng both in water and soil. The half-live of cyhalofop-butyl was 4.14 and 6.6 days in water and soil, respectively. The method was successfully applied to evaluate cyhalofop-butyl residues in water and soil applied aj. 30% emulsion, oil in water (EW) product.
마이크로파 추출법을 이용한 Negella sativa중의 휘발물질 분리: 추출물이개와 쥐의 CYP1A에 미치는 영향
박종혁 ( Jong Hyouk Park ),유학 ( Xue Liu ),김성우 ( Sung Woo Kim ),심재한 ( Jae Han Shim ) 한국환경농학회 2013 한국환경농학회 학술대회집 Vol.2013 No.-
The volatile components of Nigella sativa seeds were isolated using microwave-assisted extraction (MAE) and identified using gas chromatography. Further investigations were carried out to demonstrate the effects of wholeextracts on canine (dog) and murine (rat) cytochrome P450 1A (CYP1A). The optimal extraction conditions of MAE wereas follows: 25 mL of water, medium level of microwave oven power and 10 min of extraction time. A total of 32 compoundswere identified under the conditions using GC-FID and GC-MS. Thymoquinone (38.23%), p-cymene (28.61%), 4-isopropyl-9-methoxy-1-methyl-1-cyclohexene (5.74%), longifolene (5.33%), a-thujene (3.88) and carvacol (2.31%) werethe main compounds emitted from N. sativa seeds. Various extracts including pure compounds, essential oil, nonpolarpartition, relatively high-polar/nonpolar partition, and polar partition extracts effectively inhibited the reaction ofethoxyresorufin O-de-ethylation, which is specified for CYP1A activity both in dog and rat. This in vitro data shouldbe heeded as a signal of possible in vivo interactions. The use of human liver preparations would considerablystrengthen the practical impact of the data generated from this study.
Determination of Cyhalofop-butyl and its Metabolite in Water and Soil by Liquid Chromatography
Lina Hem(헴리나),Jeong-Heui Choi(최정희),Xue Liu(유학),Sathya Khay(카이 사티아),Jae-Han Shim(심재한) 한국농약과학회 2008 농약과학회지 Vol.12 No.4
In this study, a simple, effective, and sensitive method has been developed for the quantitative residue analysis of cyhalofop-butyl and its metabolite cyhalofop acid in water and soil when kept under laboratory conditions. The content of cyholofop-butyl and cyhalofop acid in water and soil was analyzed by first purifying the compounds through liquid-liquid extraction and partitioning followed by Silica gel (adsorption) chromatography. Upon the completion of the purification step the residual levels were monitored through high-performance liquid chromatography (HPLC) using a UV absorbance detector. The recoveries of cyhalofop-butyl from three replicates spiked at two different concentrations ranged from 82.5 to 100.0% and from 66.7 to 97.9% in water and soil, respectively. The limit of detection and minimum detection level of cyhalofop-butyl in water and soil was 0.02 ppm and lOng, respectively, The recoveries of cyhalofop acid ranged from 80.7 to 104.8% in water and from 76.9 to 98.1 % in soil. The limit of detection of cyhalofop acid was 0.005 ppm in water and 0.01 ppm in soil, while the minimum detection level was 2 ng both in water and soil. The half-live of cyhalofop-butyl was 4.14 and 6.6 days in water and soil, respectively. The method was successfully applied to evaluate cyhalofop-butyl residues in water and soil applied a.i. 30% emulsion, oil in water (EW) product.