HPLC를 이용한 아족시스트로빈과 이미다클로프리드, 메타벤즈티아주론의 토양 잔류분석 숙련도시험

김찬섭(Chan-Sub Kim),손경애(Kyeong-Ae Son),길근환(Geun-Hwan Gil),임건재(Geon-Jae Im) 한국농약과학회 2015 농약과학회지 Vol.19 No.3

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On November 2012 the testing was carried out using the soil collected and kept as the moistened state for five years, which was expected to very low residue levels of pesticides. The soil was fortified with azoxystrobin, imidacloprid and methabenzthiazuron in a manner similar to prepare soil samples for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soils treated as different levels, one of which was used to the assessment and another used to confirm. In addition, provided three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty eight institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of azoxystrobin were 48, imidacloprid and methabenzthiazuron 46.

가스크로마토그래피를 이용한 토양 중 프로사이미돈과 클로르피리포스, 메톨라클로르의 잔류분석 숙련도시험

김찬섭(Chan-Sub Kim),손경애(Kyeong-Ae Son),길근환(Geun-Hwan Gil),김진배(and Jin-Bae Kim),홍수명(Su-Myeong Hong),권혜영(Hye-Young Kwon) 한국농약과학회 2013 농약과학회지 Vol.17 No.2

The proficiency testing for the residue laboratories of pesticide registration was conducted in order to improve the reliability and the ability for pesticide residue analysis. On October 2011 the testing was carried out using the soil collected and kept as the moistened state for five years, which is expected to very low residue levels of pesticides. The soil was fortified with chlorpyrifos, metolachlor and procymidone in a manner similar to prepare soil sample for indoor soil degradation test, and then sub-samples were prepared for the distribution to participants. Some of them were randomly selected for confirm of homogeneity and to ensure the stability of samples at room temperature. Samples were consisted of two soil treated as different levels, one of which was used to the assesment and another used to confirm. In addition, provide three standard solutions, respectively concentration of 10 mg/L, and untreated soil. Forty seven institutions submitted results. The medians of results were used as the assigned values for pesticide residues. Fitness for purpose standard deviation of proficiency test was calculated by applying 20% RSD as the coefficient of variation allowed in the soil residue test. Z-score was applied for evaluation of individual pesticides, and the average of the absolute value of the Z-score for the overall assessment of pesticides. Laboratories evaluated the absolute value of the Z-score less than 2 to fit the case of chlorpyrifos and procymidone were 44, metolachlor 40.

담수처리(湛水處理)가 토양(土壤)의 인산(燐酸) 흡착(吸着) 특성(特性)에 미치는 영향(影響) I. 최대(最大) 흡착량(吸着量), 흡착(吸着) 평형상수(平衡常數) 및 흡착열(吸着熱)의 변화(變化)

김찬섭,유순호,Kim, Chan-Sub,Yoo, Sun-Ho 한국토양비료학회 1991 한국토양비료학회지 Vol.24 No.2

담수처리(湛水處理)에 의한 토양(土壤)의 환원(還元)이 토양(土壤)의 인산(燐酸) 흡착특성(吸着特性)에 어떠한 영향(影響)을 미치는지를 검토(檢討)하기 위하여 논으로 이용(利用)되어온 강서통(江西統), 밭으로 이용(利用)되어온 중동통(中東統), 및 미경작지(未耕作地)인 예산통(禮山統)을 공시토양(供試土壤)으로 하여 담수처리(湛水處理)후 인산(燐酸) 흡착(吸着) 실험(實驗)을 실시(實施) 하였다. 흡착(吸着) 실험(實驗)의 온도(溫度)는 $5{\sim}45^{\circ}C$이었으며, Langmuir 등온흡착식(等溫吸着式)과 van't Hoff식(式)을 이용(利用)하여 인산(燐酸) 최대(最大) 흡착량(吸着量)과 흡착평형상수(吸着平衡常數) 및 흡착열(吸着熱)을 구하였다. 결과(結果)를 요약(要約)하면 다음과 같다. 1. 흡착온도(吸着溫度)의 증가(增加)는 인산(燐酸)의 흡착량(吸着量)을 증가(增加) 시켰으나, 흡착(吸着) 평형(平衡)에 도달(到達)하는 속도(速度)에는 거의 영향(影響)을 미치지 못하였다. 3시간(時間)의 진탕으로 24시간후(時間後) 흡착량(吸着量)의 80~90%가 흡착(吸着)되었으며, 12시간후(時間後)에는 흡착량(吸着量)의 변화가 없었다. 2. 인산(燐酸) 최대(最大) 흡착량(吸着量)은 담수처리(湛水處理)에 의하여 강서통(江西統)은 500mgP/kg에서 850mgP/kg으로, 예산통(禮山統)은 1,850mgP/kg에서 3,300mgP/kg으로, 중동통(中東統)은 310mgP/kg에서 670mgP/kg으로 증가(增加)하였으며, 최대(最大) 흡착량(吸着量)에 대한 온도(溫度)의 효과(效果)는 거의 없었다. 3. 흡착(吸着) 평형상수(平衡常數)는 담수처리(湛水處理)에 의하여 강서통(江西統)과 예산통(禮山統)에서는 감소(減少)하였으나, 중동통(中東統)에서는 증가(增加)하였으며, 흡착온도(吸着溫度)에 따라서는 세 토양(土壤)의 값이 모두 증가(增加)하였다. 특히 점토(粘土)의 함량(含量)이 높고 토양중(土壤中) Bray 1-P의 함량(含量)이 낮은 예산통(禮山統)이 큰 값을 나타내었다. 4. Langmuir식(式)의 평형상수(平衡常數)값을 사용(使用)하여 계산(計算)한 흡착열(吸着熱)은 담수처리(湛水處理)에 의하여 강서통(江西統)은, 2.2kcal/mole에서 3.5kcal/mole로 증가(增加)하였으며, 예산통(禮山統)은 5.7kcal/mole에서 5.5kcal/mole로 거의 일정(一定)하였다. 담수(湛水)시킨 중동통(中東統)의 흡착열(吸着熱)은 4.4kcal/mole이었다. This study examines the effect of submergence on phosphorus adsorption characteristics in Gangseo(paddy soil), Yesan(non-cultivated soil), and Jungdong soil(upland soil). The soils were submerged with glucose sol'n at $28^{\circ}C$ for 17 days. After the submergence, the phosphorus adsorption was conducted at three temperatures(5, 25 and $45^{\circ}C$). The phosphorus adsorption maximum($X_m$) and the equilibrium constant(K) were obtained by Langmuir adsorption isotherm, and the heat of adsorption(${\Delta}H$) was calculated by van't Hoff's equiation. Results obtained are as follows ; 1. The amounts of adsorbed P were increased with temperature, but the effects of temperature on rate of P adsorption were very small in all three soils. 2. By submergence, $X_m$ were increased from 500mg P/kg to 850mg P/kg in Gangseo soil, from 1,850mg P/kg to 3,300mg P/kg in Yesan soil, and from 310mg P/kg to 670mg P/kg in Jungdong soil. But the effects of temperature on $X_m$ were very small in all three soils. 3. Submergence decreased K for Gangseo and Yesan soils, but increased for Jungdong soil. Whereas K were increased with temperature in all three soils. 4. By submergence, ${\Delta}H$ for Gangseo soil was greatly increased (from 2.2 Kcal/mole to 3.5 Kcal/mole), whereas that for Yesan soil changed little (from 5.7 Kcal/mole to 5.5 Kcal/mole). It was 4.4 Kcal/mole in submerged Jungdong soil.

논 토양에서 [<SUP>14</SUP>C]Butachlor의 대사시험

조유진(Yu-Jin Cho),안지영(Ji-Young An),정정훈(Jung-Hun Jung),정성훈(Sung-Hun Jung),임종수(Jong-Soo Lim),김찬섭(Chan Sub Kim),김종환(Jong-Hwan Kim) 한국농약과학회 2020 농약과학회지 Vol.24 No.1

This study was conducted to investigate the metabolic pathway and to calculate the DT<SUB>50</SUB> (halflife) and DT<SUB>90</SUB> of butachlor in the paddy soil (loam soil) which consisted of sterile and non-sterile conditions. The aerobic conditions were maintained with constant air flow in test vessels connected to the flow-through system and values for pH, dissolved oxygen, and redox potential were measured during the test period. Labelled radioactive substance (<SUB>14</SUB>C-butachlor) was used to detect the metabolites produced from the test substance. Six metabolites were found in the non-sterile soil, all less than 10% of applied radioactivity (AR) throughout the study. Of these, two main metabolites (N-(Butoxymethyl)-N-(2,6-diethylphenyl)-acetamide, N- (2,6-Diethyl-phenyl)-N-hydroxymethyl-acetamide) were identified by comparing to the authentic substance using radio-HPLC and LC-MS/MS, indicating that dechlorination, O-dealkylation occurred by microbes in the soil. The DT<SUB>50</SUB> and DT<SUB>90</SUB> values were calculated using the first-order kinetic, showing 25.3 and 84.0 days in the non-sterile soil, however those values in the sterile could not be calculated because no significant decrease was observed. Non-extractable residues increased to a maximum value of 45.6% AR at 62 days after treatment (DAT) but the volatile compounds and CO₂ were much lower levels (less than 0.5% AR). A majority of the non-extractable residue (bound residue) was associated with the humin fraction (21.2% AR) than the other fulvic acid (13.4% AR) and humic acid fraction (8.0% AR).

잔류농약 다성분 동시분석을 위한 흡착 크로마토그래피의 적용

김찬섭(Chan-Sub Kim),임양빈(Yang-Bin Ihm),최주현(Ju-Hyun Choi),이경미(Kyoung-Mi Lee),이영득(Young-Deuk Lee) 한국농약과학회 2010 농약과학회지 Vol.14 No.4

In order to develop the multi-residue purification method for 180 pesticides commonly used in Korea, many analytical methods on individual and multi- pesticide residues in the agricultural commodities and food product were examined. Through the modification of adsorption chromatographic methods used in Europe, the United States and Korea, the Florisil and silica-gel chromatographic systems were developed. Through these purification systems, elution profiles for all pesticides were examined. As the results, 145 pesticides were recovered in the range of 70-120% in Florisil clean-up system. The distribution of pesticides in the elution profile was 12 pesticides in the first fraction, 76 pesticides in the second fraction, 81 pesticides in the third fraction, 60 pesticides in the fourth fraction and 30 pesticides in the last fraction. And, in silica-gel system, 137 pesticides were recovered in the range of 70~120%. The distribution of pesticides in the elution profile was 22 pesticides in the first fraction, 59 pesticides in the second fraction, 102 pesticides in the third fraction, 46 pesticides in the fourth fraction and 8 pesticides in the last fraction.

국내등록농약의 용탈 가능성 평가

김찬섭(Chan-Sub Kim),이희동(Hee-Dong Lee),임양빈(Yang-Bin Ihm),김정한(Jeong-Han Kim),임건재(Geon-Jae Im),오병렬(Byung-Youl Oh) 한국농약과학회 2006 농약과학회지 Vol.10 No.4

Movement of pesticides applied for crop protection to the non-target environmental compartments has increasingly concerned in recent. A special review on groundwater leaching potential of pesticides registered in Korea was done by using the data submitted on half-life and adsorption of the pesticides in/on soil. Groundwater ubiquity score(GUS) of pesticides as a leaching potential was calculated by using domestic trial data on pesticide half-life in paddy or upland soils and Koc data bases of Oregon State University (OSU), British Pesticide Safety Directorate and Sweden. Of total 382 pesticides reviewed, domestic half-lives of 107 pesticides were for paddy soil and 297 pesticides for upland soil. And total 317 Koc values were collected 148 pesticides from OSU DB and 276 pesticides from UK/Sweden DB. Very highly leachable pesticides were 18 and highly leachable pesticides were 44 among 313 pesticides classified by GUS.

Dichloromethane 분배 - 흡착 크로마토그래피 - GC-ECD/NPD 분석법에 의한 토양잔류농약 다성분 분석

김찬섭(Chan-Sub Kim),이병무(Byung-Moo Lee),박경훈(Kyung-Hun Park),박병준(Byung-Jun Park),박재읍(Jae-Eup Park),이영득(Young-Deuk Lee) 한국농약과학회 2010 농약과학회지 Vol.14 No.4

Considering the efficiencies of the preparation process at each stage obtained in previous studies, the analytical determination method was established for multi-pesticide residues in soils. It consist of the acetone-extraction, the dichloromethane-partition, the Florisil or silica-gel chromatography and the gas chromatography analysis equipped with the electron capture detector and the nitrogen-phosphorus detector. In the soil recovery test by Florisil clean-up system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 165 pesticides for paddy soil, 169 pesticides for upland soil and 159 pesticides in both soils through the tested 183 pesticides. And in the soil recovery test by silica-gel system, the number of pesticides recovered in the range of 70~120% and showed less than 20% of RSD were 154 pesticides for paddy soil, 145 pesticides for upland soil, and 134 pesticides in both soils.

인공강우와 콩재배 포장 라이시메타를 이용한 diazinon과 metolachlor의 유출량 평가

김찬섭(Chan-Sub Kim),이병무(Byung-Moo Lee),박병준(Byung-Jun Park),정필균(Pil-Kyun Jung),최주현(Ju-Hyeon Choi),류갑희(Gab-Hee Ryu) 한국농약과학회 2006 농약과학회지 Vol.10 No.4

Three different experiments were undertaken to investigate the runoff and erosion loss of diazinon and metolachlor from sloped-field by rainfall. The mobility of two pesticides and which phase they were transported by were examined in adsorption study, the influence of rainfall pattern and slope degree on the pesticide losses were evaluated in simulated rainfall study, and the pesticide losses from soybean field comparing with bare soil were measured in field lysimeter study. Freundlich adsorption parameter (K) ranged 1.6~2.0 for metolachlor and 4.0~5.5 for diazinon. The K values of pesticides by the desorption method were higher than those ones by the adsorption method. Another parameter (1/n) in Freundlich equation for the pesticides tested ranged 0.96~1.02 by desorption method and 0.87~1.02 by adsorption method. By the SSLRC's classification for pesticide mobility of diazinon and metolachlor were classified as moderately mobile (75≤Koc<500). Runoff and erosion losses of pesticides by three rainfall scenarios were 0.5~1.0% and 0.1~0.7% for metolachlor and 0.1~0.6% and 0.1~0.2% for diazinon. Distribution of pesticides in soil profile were investigated after the simulated rainfall events. Metolachlor was leached to 10~15 ㎝ soil layer and diazinon was leached to 5~10 ㎝ soil layer. Losses of each pesticide in the 30% of sloping degree treatment were 0.2~1.9 times higher than those ones in the 10% of sloping degree treatment. Pesticide losses from a series of lysimeter plots in sloped land by rainfall ranged 1.0~3.1% for metolachlor and 0.23~0.50% for diazinon, and were 1/3~2.5 times to the ones in the simulated rainfall study. The erosion rates of pesticides from soybean-plots were 21~75% lower than the ones from bare soil plots. The peak runoff concentration in soybean-plots and bare soil plots were 1~9 ㎍L<SUP>-1</SUP> and 3~16 ㎍L<SUP>-1</SUP> for diazinon, 7~31 ㎍L<SUP>-1</SUP> and 5~40 ㎍L<SUP>-1</SUP> for metolachlor, respectively.

고추재배 포장 라이시메타를 이용한 fluazinam의 유출 평가

김찬섭(Chan-Sub Kim),임양빈(Yang-Bin Ihm),권혜영(Hye-Young Kwon),임건재(Geon-Jae Im) 한국농약과학회 2013 농약과학회지 Vol.17 No.4

The field lysimeter study was undertaken to investigate influence of agricultural practice and topography on runoff and erosion loss of fluazinam from the sloped land grown pepper. The WP type formulation was applied on July in 2003~2005. The wash-off rates were from 1.4% to 8.4% of the applied fluazinam. The runoff losses of fluazinam from a series of pepper grown-lysimeter plots were 0.14~0.90% in the first year, 0.01~0.04% in the second year and 0.16~0.37% in the third year for the mulched contour ridge plots, 0.47~1.59% for the mulched up-down direction ridge plots and 0.07~1.05% for the no-mulched contour ridge plots as the control, and they increased with slope degree. Concentrations of fluazinam in runoff water ranged mostly to 10 μg L<SUP>?1</SUP> at the first runoff event. Erosion rates from plots except the mulched up-down direction ridge plots was 0.00~0.21% for 10% and 20% slope-plots and 0.15~1.05% for 30% slope-plots with different slope degrees. Erosion rates from the mulched up-down direction ridge plots were 0.47~1.59% for 10% slope-plots and 0.75~1.05% for 20% slope-plots. Residues of fluazinam in soil at ten days after the application ranged from 0.007 mg kg<SUP>?1</SUP> to 0.059 mg kg<SUP>?1</SUP> except the soil under the mulch. After then the fluazinam residue in soil was dissipated at the rate of 20 days of half-life to below 0.01 mg kg<SUP>?1</SUP> at 60 days after the application.

Butachlor, ethoprophos, iprobenfos, isoprothiolane 및 procymidone의 토양 중 용탈과 이동성 예측

김찬섭(Chan-Sub Kim),박경훈(Kyung-Hun Park),김진배(Jin-Bae Kim),최주현(Ju-Hyeon Choi) 한국농약과학회 2002 농약과학회지 Vol.6 No.4

This study was conducted to investigate the downward mobility of pesticides using soil columns and to compare the experimental results with predicted values from Convective mobility test model. Five pesticides including ethoprophos, procymidone, iprobenfos, isoprothiolane, and butachlor were subjected to soil column leaching test for three types of cultivation soils. The concentrations of ethoprophos, iprobenfos, procymidone, isoprothiolane and butachlor leached from soil column of 30 em depth ranged 0.74~3.61 ㎎/ℓ, 0.36~1.67 ㎎/ℓ, 0.16~0.84 ㎎/ℓ, 0.16-0.67 ㎎/ℓ and lower than 0.15 ㎎/ℓ, respectively. Elution volume to reach the peak of ethoprophos, iprobenfos, procymidone, isoprothiolane and butachlor in the leachate ranged 2~4 PV, 3~10 PV, 5~13 PV, 4~14 PV and 19~61 PV, respectively. Convection times predicted by Convective mobility test model at standard conditions were 9~18 days for ethoprophos, 17~35 days for iprobenfos, 24~54 days for isoprothiolane, 21~65 days for procymidone and 105~279 days for butachlor, Based on these convection times, ethoprophos was classified as mobile or most mobile, isoprothiolane and procymidone as moderately mobile or mobile and butachlor as slightly mobile. On the same conditions, convection times from the model were coincided with those from soil column test in most of the soil-pesticide combinations applied. Therefore, Convective mobility test model could be applied to predict convection times of pesticides.