LC-MS와 NMR을 이용한 L-AA와 EGCG의 물리적 가공조건 상에서의 안정성 분석연구
Stability study of L-ascorbic acid and EGCG in thermal and high hydrostatic pressure process by using quantitative NMR spectroscopy and LC-MS
- 발행기관 강릉대학교·KIST 강릉분원
- 지도교수 윤정로, 엄병헌
- 발행년도 2009
- 학위수여년월 2009. 2
- 학위명 석사
- 학과 및 전공 학연협동과정
- 원문페이지 87 p.
- 본문언어 한국어
초록/요약
The aim of this study was to investigate the stability of L-ascorbic acid(L-AA) and EGCG(Epigallocatechin gallate) in thermal and high pressure process and develop the analysis method for food stability study by NMR. Most food materials should go through thermal processing for pasteurization, which inevitably induces the degradation of main useful food components such as water-soluble vitamins and tea catechins. HHP(high hydrostatic pressure) is recently introduced as alternative technology of conventional pasteurization processing, because this non-thermal technology keeps the functional materials stable and maintains its fresh flavor and texture. This emerging technology was compared with thermal treatments for evaluation of its availability. Thermal treatments were conducted in oil-bath (120℃) for 10minutes. Combined pressure and temperature treatment were performed in HHP equipment (Avure autoclave systems, INC) at pressures up to 500MPa combined with temperature (20-50℃). The quantities of L-AA, EGCG and its degradation products were measured by the quantitative NMR method and HPLC analysis method, respectively. The nuclear magnetic resonance (NMR) techniques were developed for the simultaneous quantitative analysis of L-AA and EGCG degradation. For the quantitative analysis by using NMR, several NMR experimental conditions were optimized including water-suppression techniques, acquisition (relaxation delay, acquisition time, etc) and processing methods. And sampling method with micro NMR-tube was also developed for food components stability study in normal water. The application of NMR methods in food components stability test has several advantages: rapid and simultaneous multi-components analysis method, non-destructive and accurate method. The degradation products can be analyzed without its standard compounds, which is not possible in HPLC methods. In the stability study of food components(L-AA, EGCG, Caffeine) under physical processing, L-AA increased the EGCG stability during pasteurized processing. The degradation products of EGCG induced by thermal treatment are considered as oxidant On the other hand, it is supposed that some kinds of strong antioxidants which are the degradation products of L-AA can be occurred under thermal treatment.
more목차
I. 서론 = 13
II. 재료 및 방법 = 27
1. AEC(L-AA, EGCG, CAFFEINE) 혼합용액의 준비 = 27
2. 정량분석 = 27
2-1. LC-MS/MS에 의한 AEC의 정량 및 정성분석 = 27
2-2. HPLC에 의한 정량분석 = 28
2-3. NMR에 의한 AEC의 정량 및 정성분석 = 30
3. 물리적 가공처리 = 31
3-1. 가열처리 = 31
3-1-1. AEC 200.22#0 열처리 실험 = 31
3-1-2. AEC 220.2#20 실험 = 32
3-2. 초고압처리 = 32
3-3. Sonication 처리 = 32
III. 결과 및 고찰 = 33
1. HPLC와 LC-MS에 의한 정량분석 = 33
1-1. AEC용액의 HPLC Chromatogram = 33
1-2. 각 성분에 대한 HPLC에서의 UV/Vis spectrum = 39
1-3. LC-MS/MS에서의 각 성분에 대한 MS spectrum = 41
2. NMR을 이용한 AEC의 정량분석 방법설정 = 44
2-1. NMR sampling 방법의 최적화 = 44
2-2. NMR parameter의 최적화 = 47
2-3. Water-suppression technique의 최적화 = 50
3. NMR을 이용한 AEC solution의 안정성 연구 = 52
3-1. AEC 용액의 보존성 연구 = 52
3-2. AEC solution의 NMR 분석 = 59
4. 물리적 가공처리 공정에서의 AEC의 안정성 연구 = 70
4-1. 상온 및 SONICATION에 의한 안정성 평가 = 70
4-2. 열처리에 의한 안정성 연구 = 72
4-2-1. AEC 농도 별 열처리 실험 = 72
4-2-2. AEC 220.22#0 열처리 실험 = 75
4-2-3. AEC의 EGCG 농도변화 별 열처리 실험 = 77
4-2-4. AEC 220.2#20 실험 = 80
4-3. 압력처리에 의한 안정성 연구 = 83
IV. 결론 = 85
V. 참고문헌 = 86
