동위원소희석 액체크로마토그래피 질량분석법을 이용한 종합영양제와 분유 중 비타민 B5와 비타민 B6 분석

다국어 초록 (Multilingual Abstract)

An isotope dilution liquid chromatography/mass spectrometry (ID-LC/MS) method was developed for the accurate simultaneous determination of vitamin B5 and vitamin B6 in multivitamin tablets and infant formula. As internal standards, 13C3,15N1-pantothenic acid and 13C4-pyridoxine were spiked to both multivitamin tablets and infant formula. Multivitamin tablets were extracted distilled with water for 3 hours at 4 ℃ and infant formula was extracted with acetonitrile. The chromatographic analysis was carried out using gradient elution with a Waters X-bridge C18 column and the mobile phase consisted of 0.1 % formic acid in water and methanol. The mass spectrometer was operated in selected ion monitoring mode to monitor the collisionally induced dissociation channels, m/z170→152 for pyridoxine, m/z174→156 for 13C4-pyridoxine, m/z168→150 for pyridoxal, m/z169→152 for pyridoxamin, m/z220→90 for pantothenic acid and m/z224→94 for 13C3,15N1-pantothenic acid. The repeatability and reproducibility tests of the ID-LC/MS method in multivitamin tablets and infant formula showed less than 2.0 % of relative standard deviation. This method was applied to the analysis of commercial products such as multivitamins and cereal. This ID-LC/MS method has established candidate reference method for accurate determination of pantothenic acid and pyridoxine in multivitamin tablets and infant formula.

목차 (Table of Contents)

• Ⅰ. 서론 1
• 1. 연구배경 1
• 1) 비타민 B 복합체 1
• 2) 판토텐산 2
• 3) 피리독신 5
• 2. 연구목적 8
• 3. 동위원소희석 액체크로마토그래피-질량분석법 10
• 1) 액체크로마토그래피 10
• 2) 질량분석법 11
• 3) 동위원소희석 질량분석법 12
• Ⅱ. 재료 및 실험방법 16
• 1. 시약 및 재료 16
• 2. 기기 및 장치 17
• 3. 실험방법 18
• 1.1.1. 표준용액 제조 18
• 1.1.2. 종합영양제 시료 전처리 20
• 1.1.3. 분유 시료 전처리 21
• 4. 분석조건 22
• 1) 고성능 액체크로마토그래피 22
• 2) 질량 분석기 24
• Ⅲ. 결과 및 고찰 27
• 1. 질량스펙트럼 27
• 1) Full scan 질량스펙트럼 27
• 2) Product ion 질량스펙트럼 31
• 2. LC-MS와 LC-MS/MS 분석 35
• 3. 시료 전처리 최적화 39
• 1) 종합영양제 시료 전처리 최적화 39
• 2) 분유 시료 전처리 최적화 41
• 4. 분석법 검증 47
• 1) 종합영양제 중 판토텐산과 피리독신 동시 분석법 검증 47
• 2) 분유 중 판토텐산과 피리독신 동시 분석법 검증 50
• 3) 검출한계 51
• 5. 시중에 판매되는 식품 중 판토텐산과 피리독신 함량 분석 54
• Ⅳ. 결론 60
• Ⅴ. 참고문헌 62
• ABSTRACT 64