보고서 정보
주관연구기관 |
국립과학수사연구원 National Forensic Service |
보고서유형 | 최종보고서 |
발행국가 | 대한민국 |
언어 |
한국어
|
발행년월 | 2013-12 |
과제시작연도 |
2013 |
주관부처 |
미래창조과학부 Ministry of Science, ICT and Future Planning |
과제관리전문기관 |
국립과학수사연구원 National Forensic Service |
등록번호 |
TRKO201400012141 |
과제고유번호 |
1315000558 |
사업명 |
중장기과학수사감정기법연구개발 |
DB 구축일자 |
2014-07-05
|
키워드 |
메소밀.엔도설판.글리포세이트.글루포시네이트.농약.methomyl.endosulfan.glyphosate.glufosinate.pesticide.
|
DOI |
https://doi.org/10.23000/TRKO201400012141 |
초록
▼
◯ 다양한 액상 매질(생수, 맥주, 소주, 막걸리 및 요구르트) 중 자주 검출되는 methomyl, endosulfan, glyphosate 및 glufosinate의 추출방법을 가스크로마토그래피/질량분석기로 확립. Glyphosate 및 glufosinate는 유도체화를 거쳐 가스크로마토그래피/질량분석기로 분석. 2008년-2011년 의뢰된 농약 관련 사건 액상 압수품 중 농약의 정량 실시
◯ 각기 다른 매질 속에서 methomyl, endosulfan, glyphosate 및 glufosinate를 확인하고 각 매질 중 L
◯ 다양한 액상 매질(생수, 맥주, 소주, 막걸리 및 요구르트) 중 자주 검출되는 methomyl, endosulfan, glyphosate 및 glufosinate의 추출방법을 가스크로마토그래피/질량분석기로 확립. Glyphosate 및 glufosinate는 유도체화를 거쳐 가스크로마토그래피/질량분석기로 분석. 2008년-2011년 의뢰된 농약 관련 사건 액상 압수품 중 농약의 정량 실시
◯ 각기 다른 매질 속에서 methomyl, endosulfan, glyphosate 및 glufosinate를 확인하고 각 매질 중 LOD, LOQ, 검량선, matrix effect, extraction recovery, process efficiency, accuracy 및 precision 결과 얻음.
◯ Methomyl은 매질에 대한 영향을 많이 받아 추출효율이 양호하지 않았고, endosulfan sulfate는 매질에 의한 영향을 거의 받지 않아 추출효율이 양호하였음.
Abstract
▼
* Intentionally or accidentally added pesticides in soft drinks, alcoholic beverages and bottled water commonly encountered in everyday life has to be detected quickly, provide the clue to the scientific investigation and make emergency center deal with pesticide- related poison quickly.
The purp
* Intentionally or accidentally added pesticides in soft drinks, alcoholic beverages and bottled water commonly encountered in everyday life has to be detected quickly, provide the clue to the scientific investigation and make emergency center deal with pesticide- related poison quickly.
The purpose of this study was to establish the extraction method for methomyl, endosulfan, gly phosate and glufosinate frequently detected pesticides, in liquid evidence and investigate the matrix effect, extraction recovery, process efficiency, accuracy and precision in various matrixes (water, beer, soju (Korean distilled spirits), rice wine, and yogurt).
Methomyl and endosulfan sulfate in liquid matrix were prepared by 4 types of liquid-liquid extraction (LLE) methods: Method 1 (acidic-alkali extraction using ethylacetate), Method 2 (ethylacetate-ethylacetate extraction, Method 3 (ethylacetate-hexane extraction) and Method 4(ethylacetate-dichloromethane extaction). Process efficiency of Method 1 was satisfactory. The residue after extraction was reconstituted in 100 μL of methanol and analyzed using Gas chromatography–mass spectrometry (GC/MS). Glyphosate and glufosinate in liquid matrix were prepared by Solid Phase Extraction (SPE) and the residue after extraction was derivatized with trifluoroacetic acid and trifluoroethanol. The residue after evaporation was reconstituted in 100 μL of methanol and analyzed using GC/MS.
The limit of detection, quantification (LOD and LOQ) and calibration curve were determined for methomyl, endosulfan sulfate, glyphosate and glufosinate in all matrix.
The matrix effect and process efficiency of methomyl in water, beer, soju, rice wine and yogurt matrix were not good while those of endosulfan sulfate in water, beer, soju, rice wine and yogurt matrix were relatively good. Therefore, methomyl was vulnerable to matrix. The matrix effect and process efficiency of glyphosate in water and soju were extremely bad but those in beer were good. The matrix effect and process efficiency of glufosinate in water and soju were good. The accuracy and precision were within 15% for methomyl, endosulfan sulfate, glyphosate and glufosinate in all matrix.
Among evidences collected from the Western District Office of National Forensic Service Between 2008-2012, there were methomyl-related cases (n=27) in which the concentrations of methomyl in various matrixes ranged 1.8-73.8 mg/mL (mean 19.02), endosulfan -related cases (n=8) in which the concentrations of endosulfan in various matrixes ranged 0.2-13.05 mg/mL (mean 2.97), and glyphosate-related cases (n=6) in which the concentrations of glyphosate ranged 0.095-0.7mg/mL (mean 0.40).
The matrix effect, extraction recovery and process efficiency depended on the characteristics of the pesticides and liquid matrix and varied largely. This study will be useful and applicable to the analysis of other pesticides from liquid evidences in forensic cases.
목차 Contents
- 연구사업 최종보고서 ... 1
- 성과요약문 ... 2
- Summary ... 4
- 목차 ... 5
- 제1장 연구개발과제의 개요 ... 6
- 제1절 연구개발과제의 목표 ... 6
- 제2절 연구개발과제의 필요성 ... 7
- 제2장 연구개발과제의 국내.외 연구개발 현황 ... 8
- 제 1절: 국내.외 관련분야에 대한 기술개발 현황 ... 8
- 제 2절: 연구결과가 국내.외 기술개발 현황에서 차지하는 위치 ... 8
- 제3장 연구개발과제의 연구수행 내용 및 결과 ... 9
- 제 1절: 추진 전략, 연구방법 및 추진체계의 개요 ... 9
- 제 2절: 연구방법 및 결과 ... 10
- 제4장 목표달성도 및 관련분야에의 기여도 ... 28
- 제5장 연구개발결과의 활용계획 ... 29
- 제1절 활용성과 ... 29
- 제2절 활용계획 ... 30
- 제6장 참고문헌 ... 31
- 제7장 첨부서류 ... 33
- 끝페이지 ... 33
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