농산물 중 극성 유기인계 살충제의 잔류분석법 개발

이영득 ( Young Deuk Lee ) 한국환경농학회 2016 한국환경농학회 학술대회집 Vol.2016 No.-

An analytical method was developed to determine residues of polar organophosphorus insecticides including azamethiphos, demeton-S-methyl, dicrotophos, oxydemeton-methyl and a major metabolite, demeton-S-methyl sulfone in agricultural products for the inspection of agricultural foods. Total of five representative types of agricultural commodities which comprised brown rice, mandarine, green pepper, potato and soybean were selected for validation of the method. Target analytes were simultaneously extracted with acetone from raw or moistened samples. The extract was diluted with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives while the analyte remained in the aqueous phase. Dichloromethane partition was then followed to recover all the analytes from the aqueous phase. Florisil or weak anion-exchange column chromatography was employed to further purify the extract prior to determination by gas-liquid chromatography (GLC). A temperature-programmed GLC using a polar capillary column was successfully applied to separate and quantitate each residue of the analyte in sample extracts with nitrogen-phosphorus detection. Internal standardization was additionally applied to minimize variation during the instrumental quantitation. A confirmatory and/or alternative quantitative method was also provided using GLC coupled with the mass spectrometric technique.

식품의약품안전처 SESSION : 식품 중 잔류농약 위해도 결정 및 안전역 확보를 위한 연구

이영득 ( Young Deuk Lee ) 한국환경농학회 2013 한국환경농학회 학술대회집 Vol.2013 No.-

총 섭취 식품의 80%를 차지하는 농산물을 안정적으로 생산하기 위하여 현대 농업에서 농약의 사용은 필수불가결하다. 농작물 재배 중 해충 방제 효율을 확보하기 위해서는 농약의 특성별로 살 포 시기 및 횟수를 일정 수준 허용하여야 하므로 농산물 중 잔류농약에 의한 위해 유발 가능성은 필연적이며 농약별로 잔류 수준의 변이 폭은 상당히 크게 나타난다. 각 농약별 만성독성학적 안전 성 척도인 ADI는 잔류농약에 의한 위해성의 상한선이다. 잔류 수준과 ADI 사이에서 실용적으로 안전성을 확보하는 수단으로 잔류허용기준이 설정되고 있으며 이론적으로 산출되는 TMDI가 ADI 를 초과하지 않는 범위로 관리되고 있다. 그러나 국내에서는 이러한 잔류허용기준을 농약 및 작물 별로 다수의 작물잔류성 시험결과로부터 산출된 통계적 유의성에 근거하여 설정하지는 못하고 있다. 즉, 단일 작물잔류성 시험결과를 단순히 타 국가의 허용기준과 비교하거나 임의의 변이성을 부 여, round-up하는 소위 전문가들의 eyeball method에 근거하여 설정하고 있다. 그렇다고 국제적으로 인정되는 통계적 유의성을 확보하기 위하여 작물잔류성 시험수를 대폭 늘리는 것도 현실적으로 매우 어렵다. 따라서 국제적으로 최소기준을 만족하면서 국내 연구실정에 부합되는 적절한 잔류허 용기준의 설정체계가 요구된다. 다행히 국토 면적이 좁고 기후대가 편중되어 있으며 농약 사용에 대한 관리 체계가 비교적 잘 정비되어 있는 점을 효과적으로 이용할 수 있다. 따라서 소실속도에 따른 농약군 및 대표 작물을 지역별 GAP 관리에 따라 작물잔류성 시험을 수행하고 이러한 시험결과로부터 보편적으로 통용될 수 있는 통계학적 분산 척도를 산출, 적용한다면 보다 과학적으로 안 전성이 확보된 잔류허용기준 설정 체계를 수립할 수 있을 것이다. 본 연구에서는 이러한 최종 잔류수준에 영향을 미치는 주요 인자를 제안하고 지역 및 기후대별 통계학적 실험설계를 고안함과 동시에 잔류자료의 해석 및 새로운 허용기준 설정체계를 위한 연구방향을 제시하고자 하였다.

농산물 중 살충제 Etofenprox의 잔류분석법

이영득 ( Young Deuk Lee ),모에닌퓨 ( Moe Hnin Phyu ),임무혁 ( Moo Hyeog Im ) 한국환경농학회 2008 한국환경농학회 학술대회집 Vol.2008 No.2

동위원소 표지 내부표준법을 이용한 축산물 중 산성 제초제의 정밀 잔류분석법 개발

이영득 ( Young Deuk Lee ) 한국환경농학회 2019 한국환경농학회 학술대회집 Vol.2019 No.-

An analytical method was developed to simultaneously determine residues of acidic herbicides/PGRs including active ingredients, their esters and conjugates in livestock products for the official purpose. Total of five representative types of animal commodities which comprised meat, pork, chicken, egg and milk were selected for validation of the method. Prior to extraction, the sample was alkaline-hydrolyzed to liberate parent ingredients from their esters and conjugates. After acidification to ion-suppress the acidic moiety, all of target analytes were extracted with acetonitrile from samples, and then followed by partition under increased ionic strength in the aqueous phase. Polymer-based solid-phase extraction was employed to further purify the extract. Each analyte was separated on an octadecylsilyl column in liquid chromatography and determined by tandem mass spectrometry using the selected-reaction monitoring technique. To enhance the precision of quantitation during the whole analytical procedure, deuterium or 13C-labeled standards were adopted in situ for the internal standardization, which could accurately compensate both the instrumental fluctuation by matrix effects and the extraction/purification efficiency.

잔류허용기준의 국제적 조화를 위한 작물잔류성 시험 방법 및 자료 해석의 합리화

이영득 ( Young Deuk Lee ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-

A procedural and policy-oriented research was undertaken to fulfill the local maximum residue limits (MRLs) of pesticide residues to the international standards. Scientific basis and criteria for the evaluation of supervised trial dataset to establish local MRLs were precisely compared with MRL calculation systems of Codex, EU and USA, which operated under non-distributional statistical approximations. Practical approach and improvement in pursuit of local implementation was studied to harmonize the local MRL setup system to the international standards in compliance with minimal statistical requirements including number of independent trials, production and handling of residue data along with application of extrapolation cases and food processing factors. Trial guidelines of pesticide residues comprising field and analytical good-laboratory practices (GLPs) were also concisely inspected to produce reliable residue data scientifically applicable to MRL calculation. Manuals with concise standard operating procedures during supervised trials and reporting format for the submission were concurrently provided to readily access the internationally-approved data production.

농산물 중 Methomyl 및 전구체 살충제의 동시 잔류분석법 개발

이영득 ( Young Deuk Lee ) 한국환경농학회 2017 한국환경농학회 학술대회집 Vol.2017 No.-

An analytical method was developed to simultaneously determine residues of methomyl and its precursor insecticides including alanycarb and thiodicarb in agricultural products for the official purpose. All of target analytes were extracted with methanol from raw or moistened samples. To the extract was added hydrochloric acid to hydrolyze alanycarb. Methomyl was quantitatively evolved from alanycarb within 10 min, while intact methomyl and thiodicarb were stable up to 1 hr in the acidic media. The hydrolyzate was diluted with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives while the analyte remained in the aqueous phase. Enhancing ionic strength of the aqueous phase, dichloromethane partition was then followed to recover methomyl and thiodicarb. Florisil and/or weak anion-exchange column chromatography were employed to further purify the extract prior to determination by high-performance liquid chromatography (HPLC) with detection of ultraviolet absorption at 234 nm. Linear gradient elution of acetonitrile/water mixture on an octadecylsilyl column was successfully applied to separate each residue of the analyte. Total of five representative types of agricultural commodities which comprised brown rice, mandarine, green pepper, potato and soybean were selected for validation of the method. A confirmatory and/or alternative quantitative method were also provided using LC coupled with the mass spectrometric technique.

농산물 중 Sulfonylurea계 제초제의 공정 잔류분석법 개발

이영득 ( Young Deuk Lee ) 한국환경농학회 2018 한국환경농학회 학술대회집 Vol.2018 No.-

An analytical method was developed to simultaneously determine residues of four sulfonylurea herbicides including chlorimuron-ethyl, ethametsulfuron-methyl, rimsulfuron and tribenuron-methyl in agricultural products for the official purpose. All of target analytes were extracted with acetonitrile containing 0.5 M ammonium chloride from raw or moistened samples. The extract was diluted with saline water, and subjected to n-hexane washing to remove nonpolar co-extractives while the analyte remained in the aqueous phase. Enhancing ionic strength of the aqueous phase, dichloromethane partition was then followed to recover all the analytes. Weak anion-exchange column chromatography using SPE-aminopropyl cartridge was employed to further purify the extract prior to determination by high-performance liquid chromatography (HPLC) with detection of ultraviolet absorption at 234 nm. Linear gradient elution of acetonitrile/phosphate buffer (pH 3.0) mixture on an octadecylsilyl column was successfully applied to separate each residue of the analyte. Total of five representative types of agricultural commodities which comprised brown rice, mandarine, green pepper, potato and soybean were selected for validation of the method. A confirmatory and/or alternative quantitative method were also provided using LC coupled with the mass spectrometric technique.

수상강연 : 학술상 ; 잔류농약 공정 분석법의 확립 및 표준화

이영득 ( Young Deuk Lee ) 한국환경농학회 2009 한국환경농학회 학술대회집 Vol.2009 No.2

식품의약품안전처 SESSION : 농산물 중 비극성 살응애제의 잔류분석법

이영득 ( Young Deuk Lee ),조범석 ( Beom Seok Cho ) 한국환경농학회 2013 한국환경농학회 학술대회집 Vol.2013 No.-

대표 농산물을 대상으로 bromopropylate, chlorfenapyr, etoxazole, pyrimidifen, spirodiclofen 등 비극성 살응애제 5종에 대한 공정 잔류분석법을 개발하고자 하였다. 통합적으로 분석용 시료를 조 제하되 각 성분들은 개별적으로 정밀 정량함으로써 분석의 효율성을 높임과 동시에 잔류허용기준 의 위반 여부를 명확히 판별할 수 있는 개별 분석법을 확립하였다. 적용 농산물 군의 대표 농산물 로서 현미, 사과, 감귤, 고추, 배추의 5종을 선정하였으며 각 함수 시료로부터 대상 성분들을 acetonitrile로 동시에 추출하였다. 추출물을 흡인 여과한 후 농축 과정 없이 다량의 식염수로 희석 한 후 직접 비극성 용매로 분배 추출하였으며 유지 함유 시료는 n-hexane-acetonitrile 분배법을 추 가하여 비극성 방해물질을 제거하였다. 분배 추출액은 Florisil column chromatography로 최종 정 제하여 기기분석에 공시하였다. Bromopropylate, chlorfenapyr, pyrimidifen 및 spirodiclofen은 GLC/ECD, etoxazole 및 pyrimidifen은 GLC/NPD와 HPLC/UVD를 적용하여 최적 기기분석 조건을 설정하였다. 확립된 시료 조제 및 기기분석법의 결과 무처리 농산물 시료 중 간섭물질은 관찰되지 않았다. 분석법 검증실험의 결과, 잔류분석기준인 정량한계 0.05 mg/kg 이하 및 허용기준의 1/2과 회수율 70∼120% 이내를 충분히 만족하였으며 분석오차는 대상 농약과 농산물 시료에 상관없이 10% 이내였다. 시료 중에서 검출된 잔류분에 대한 정성적 신뢰성을 확보하기 위하여 추가의 크로 마토그래피법과 질량분석기을 이용한 재확인법을 제시하였다.

토양중 [ 14C ] Carbofuran 의 분해 및 비추출성 잔류분의 특성

이영득(Young Deuk Lee),박창규(Chang Kyu Park) 한국응용생명화학회 1995 Applied Biological Chemistry (Appl Biol Chem) Vol.38 No.3

A study was undertaken to compare degradation patterns of carbofuran in soils between submerged and upland moisture conditions. [3-^(14)C]Carbofuran was treated in each soils at the rate of 1.0 ㎎/㎏ (87.8 kBq ^(14)C/50 g soil) and the time-course analysis for distribution of radioactivity and degradation products were conducted. Differences in the pathway and rate of carbofuran degradation in soils were observed between submerged and upland moisture conditions, major degradation being hydrolysis at 7-C position and oxidation at 3-C position, respectively. Carbofuran showed less persistence in soils of higher moisture contents. A significant portion, 24∼39% of the total radioactivity, resided in soils as nonextractable residues at 60 days after treatment. The nonextractable radioactivity was mainly located in soil organic matter, fulvic acid, humic acid and humin fractions. Gel filtration chromatography confirmed the incorporation of carbofuran and its degradation products into the organic matter.