지원사업
학술연구/단체지원/교육 등 연구자 활동을 지속하도록 DBpia가 지원하고 있어요.
커뮤니티
연구자들이 자신의 연구와 전문성을 널리 알리고, 새로운 협력의 기회를 만들 수 있는 네트워킹 공간이에요.
논문 기본 정보
- 자료유형
- 학위논문
- 저자정보
- 지도교수
- 이계호
- 발행연도
- 2015
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2015
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An isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS) was developed for the accurate determination of cholesterol in infant formula. As internal standard, cholesterol-D4 was spiked to infant formula. In order to release cholesterol out of cholesteryl ester, saponification was carried out. Saponification conditions were optimized according to heating temperature, heating time and KOH mol.
From the results, the optimum conditions were as follows ; heating temperature 70℃, heating time 180 min, and 8 M KOH 0.8 mL for a 0.1 g infant formula sample. The separation of cholesterol was carried out uisng liquid-liquid extraction. The chromatographic analysis was carried out by Phenomenex Kinetex C18 column. The mobile phase was 0.1% acetic acid in Methanol/Water (99/1), and flow rate was 0.3 mL/min. Cholesterol and cholesterol-D4 were monitored at mass transfer m/z 369 → 259 and 373 → 263 respectively. The reproducibility of the method was evaluated to be 0.25 % of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9 % within a 95% confidence level. The standard reference materials, NIST SRM 1849a, having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM 1849a within the uncertainty.
From the results, the optimum conditions were as follows ; heating temperature 70℃, heating time 180 min, and 8 M KOH 0.8 mL for a 0.1 g infant formula sample. The separation of cholesterol was carried out uisng liquid-liquid extraction. The chromatographic analysis was carried out by Phenomenex Kinetex C18 column. The mobile phase was 0.1% acetic acid in Methanol/Water (99/1), and flow rate was 0.3 mL/min. Cholesterol and cholesterol-D4 were monitored at mass transfer m/z 369 → 259 and 373 → 263 respectively. The reproducibility of the method was evaluated to be 0.25 % of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9 % within a 95% confidence level. The standard reference materials, NIST SRM 1849a, having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM 1849a within the uncertainty.
목차
Ⅰ. 서론 11. 연구배경 1(1) 콜레스테롤의 특성 3(2) 선행연구 52. 동위원소희석 액체크로마토그래피 질량분석법 6(1) 동위원소희석 질량분석법 6(2) 액체크로마토그래피 9(3) 질량분석법 11Ⅱ. 실험 131. 시약 및 재료 132. 기기 및 장치 143. 실험방법 153.1 표준용액 제조 15(1) 일차표준용액 제조 15(2) 동위원소물질 표준용액 제조 15(3) 동위원소비 표준용액 제조 163.2 시료 전처리 174. 분석조건 18(1) 고성능 액체크로마토그래피 18(2) 질량분석기 205. 농도계산 22Ⅲ. 결과 및 고찰 231. 질량스펙트럼 232. 액체크로마토그래피 질량분석기의 측정 253. 시료 전처리 최적화 28(1) 비누화반응 최적화 304. 액체크로마토그래피 질량분석법의 검증 34(1) 반복성과 재현성 34(2) 표준물질의 검증 36Ⅳ. 결론 38Ⅴ. 참고문헌 39Ⅵ. Abstract 42
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