지원사업
학술연구/단체지원/교육 등 연구자 활동을 지속하도록 DBpia가 지원하고 있어요.
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연구자들이 자신의 연구와 전문성을 널리 알리고, 새로운 협력의 기회를 만들 수 있는 네트워킹 공간이에요.
논문 기본 정보
- 자료유형
- 학위논문
- 저자정보
- 지도교수
- 李奎承
- 발행연도
- 2013
- 저작권
- 충남대학교 논문은 저작권에 의해 보호받습니다.
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초록· 키워드
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Polar pesticides like pymetrozine(log Pow: -0.18) are known to be difficult to analyze. However, several methods have been developed for determination of pymetrozine.
The analytical method of pymetrozine using hydromatrix set by KFDA(Korea Food & Drug Administration) has difficulty in terms of quantification. Therefore, precise single residue analytical method was developed for representative crops using liquid-liquid extraction(LLE). The pymetrozine residue was extracted with methanol from 11 representative crops such as apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified by liquid-liquid partition(LLE) and silica solid phase extraction(SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using C8 column. LOQ(limit of quantitation) of pymetroizinie was 1 ng (S/N>10) and MQL(method quantitation limit) was 0.01 mg/kg. Mean recoveries of 11 crop samples fortified with three different levels(MQL, 10×MQL and 50×MQL) were in the range of 83.1∼98.5% with coefficients of variation(CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.
The analytical method of pymetrozine using hydromatrix set by KFDA(Korea Food & Drug Administration) has difficulty in terms of quantification. Therefore, precise single residue analytical method was developed for representative crops using liquid-liquid extraction(LLE). The pymetrozine residue was extracted with methanol from 11 representative crops such as apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified by liquid-liquid partition(LLE) and silica solid phase extraction(SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using C8 column. LOQ(limit of quantitation) of pymetroizinie was 1 ng (S/N>10) and MQL(method quantitation limit) was 0.01 mg/kg. Mean recoveries of 11 crop samples fortified with three different levels(MQL, 10×MQL and 50×MQL) were in the range of 83.1∼98.5% with coefficients of variation(CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.
목차
Ⅰ. 서론 1Ⅱ. 재료 및 방법 81. 시험약제, 시약 및 기구 82. 실험방법 102.1 기존 고시 분석법 검정 102.2 선행 연구방법의 적용 112.3. Pymetrozine 분석방법 연구 122.3.1 대표작물 선정 122.3.2 기기분석 조건 152.3.3 Pymetrozine의 검출한계 및 정량한계 측정 162.3.4 재현성 검정 162.3.5 표준검량선 작성 162.3.6 정제조건 비교시험 162.3.6.1 Silica gel column을 이용한 정제 162.3.6.2 Silica SPE cartridge를 이용한 정제 172.3.7 분배조건별 분배효율 비교시험 172.3.8 추출조건 확립 182.3.9 분석정량한계 192.3.10 개선 분석법의 검증 20Ⅲ. 결과 및 고찰 211. 기존 고시 분석법의 회수율 212. 선행 연구방법 적용 시 회수율 243. 분석기기의 검출한계, 정량한계 및 재현성 254. 검량선의 직선성 확인 275. Silica 흡착 크로마토그래피 정제조건의 확립 296. 분배조건 확립 337. 추출조건 확립 368. 분석정량한계 399. Pymetrozine 분석방법의 확립 3910. 개선 분석법의 검증 42Ⅳ. 결론 50Ⅴ. 참고문헌 51ABSTRACT 56
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