GCB/NH2 이중층고체상추출을 이용한 농약잔류 다성분동시분석법의 정제 효율 평가

다국어 초록 (Multilingual Abstract)

The efficiency of dual-layer solid-phase extraction(graphitized carbon/NH2 SPE), sorbents characterized by different mechanisms of sorption, was evaluated in view of sample clean-up procedure of multiresidue method(MRM).
Individually graphitized carbon block(GCB) and aminopropyl(NH2) SPE were evaluated with several clean-up solvent systems. Suitable elution solvents were selected toluene for GCB SPE and acetone, ethylacetate for NH2 SPE. Then selected solvents were mixed to various ratio and tested as a GCB/NH2 dual-layer SPE eluent.
Suitable elution solvents for 40 pesticides with a wide range of polarity were studied 65% ethyl acetate/toluene, 70% acetone/toluene. Two solvents were compared in clean-up for lettuce. As a result, 65% ethyl acetate/toluene was showed more efficiency to remove sample matrix and selected most appropriate elution solvent for clean-up of GCB/NH2 dual-layer SPE.
The solvent of 65% ethyl acetate/toluene was showed over 90% of recovery in almost pesticides, but some polar pesticides such as clothianidin, thiamethoxam, and carbendazim were eluted insufficiently.
And cymoxanil, pyroquilon, thiacloprid and boscalid were affected by matrix co-extractives in low level test. Nevertheless, these pesticides also showed 90~110% recovery reducing the affection of co-extractives of sample matrix by HPLC/MS analysis.

목차 (Table of Contents)

• Ⅰ. 서론 1
• Ⅱ. 재료 및 방법 7
• 1. 실험재료 7
• 1.1 대상 시료 및 조제 7
• 1.2 시약 7
• 1.2.1 실험 대상 농약 성분 7
• 1.2.2 시약 13
• 1.3 고체상추출 및 기기분석 13
• 1.3.1 고체상추출(SPE) 13
• 1.3.2 분석장비 13
• 1.3.2.1 HPLC/UVD 분석조건 13
• 1.3.2.2 HPLC/FLD 분석조건 14
• 1.3.2.3 HPLC/MSD 분석조건 15
• 2. 실험방법 17
• 2.1 전처리분석법 정립 17
• 2.1.1 시료 전처리 방법 17
• 2.1.2 이중층고체상추출 정제방법 17
• 2.1.2.1 GCB, NH₂ SPE 단일 용출용매 17
• 2.1.2.2 GCB/NH₂ 이중층고체상 혼합용출용매 18
• 2.1.2.3. GCB/NH₂ 이중층고체상 혼합용출용매의 정제효율 비교 18
• 2.1.3 다양한 시료 별 GCB/NH₂ 이중층고체상 정제효율 18
• 2.1.4 GCB/NH₂ 이중층고체상의 정제 회수율 19
• 2.2 HPLC/MS를 이용한 matrix effect 제거 19
• 2.2.1 개별 농약 성분의 이온 선정 19
• 2.2.2 선택이온(SIM) 분석법을 이용한 시료 불순물 제거 20
• Ⅲ. 결과 및 고찰 21
• 1. 전처리 분석법 정립 21
• 1.1 GCB/NH₂ 이중층고체상 용출용매 선발 21
• 1.1.1 GCB, NH₂ SPE 단일 용출용매 선발 21
• 1.1.2 GCB/NH₂ 이중층고체상 혼합 용출용매 선발 26
• 1.1.3 GCB/NH₂ 이중층고체상 혼합 용출용매의 정제효율 비교 31
• 1.2 시료에 따른 GCB/NH₂ 이중층고체상 정제효율 34
• 1.3 GCB/NH₂ 이중층고체상의 정제 회수율 37
• 2. HPLC/MS를 이용한 matrix effect 감소 42
• 2.1 개별 농약 성분의 이온 선정 42
• 2.2 HPLC/MS를 이용한 matrix effect 감소 44
• Ⅳ. 결론 46
• Ⅴ. 참고문헌 48
• ABSTRACT 52