본 연구는 건강기능식품 프랑스해안송껍질추출물 중 catechin, caffeic acid, ferulic acid, taxifolin에 대한 동시분석법을 개발하는 연구이다. 최적분석조건을 확립하기 위해 시료 채취량, 용매 조건을 비교 검토하였으며, UPLCMS/ MS를 이용하여 각 4개 성분에 대한 정확한 분석 및 분석시간의 효율성도 향상하였다. 분석 시 사용한 컬럼은 Acquity UPLC BEH C18이며, 정량이온으로 catechin, caffeic acid, ferulic acid, taxifolin 각각 133, 135, 245 및 248을 선정하였다. 확립된 시험법에 대해 특이성, 직선성, 검출한계, 정량한계, 정확성, 정밀성 등의 밸리데이션을 수행하였다. 4개 성분 모두 50-25000 mg/L 농도에서 결정계수(R2) 0.999이상으로 높은 직선성을 확인하였다. 또한 회수율은 84.9-104%이었고, 정밀성은 1.2-4.3%의 RSD를 확인하였다. 개발된 시험법은 프랑스해안송껍질추출물 중 catechin, caffeic acid, ferulic acid, taxifolin 분석을 위한 시험법으로 활용되기에 적합한 것으로 판단된다.

This study was conducted to develop a simultaneous analysis method for ferulic acid, caffeic acid, catechin and taxifolin from Health Functional Food (HFF) Pinus Pinaster bark extract. The simultaneous analytical method for ferulic acid, caffeic acid, catechin and taxifolin is carried out using UPLC-MS/MS. The method validation was performed to determine selectivity, linearity, accuracy, limit of detection (LOD), limit of quantification (LOQ) and precision for ferulic acid, caffeic acid, catechin and taxifolin. LC-MS/MS method was established using an Acquity UPLC BEH C18 Column and was applied for these 4 compounds. Product-ion traces, at m/z 194.2 → 133, 180.2 → 135, 290.3 → 245, 304.3 → 248, were used for quantitative analysis of ferulic acid, caffeic acid, catechin and taxifolin, respectively. Excellent linearity (r2=0.999) was observed for ferulic acid, caffeic acid, catechin and taxifolin in the concentration range (50-2500 mg/L). The observed recoveries of these 4 compounds were found to be between 84.9 and 104.9%, while precision was between 1.20 and 4.43% relative standard deviation (% RSD).

ABSTRACT
Materials and Methods
    시약 및 재료
    표준용액 조제
    최적분석조건 확립
    밸리데이션 방법
    기기조건
Results and Discussio
    최적분석조건 확립
    밸리데이션 및 적용성
국문요약
References

• 오재명(식품의약품안전처 영양기능연구팀) | Jae-Myoung Oh (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation)
• 김지안(식품의약품안전처 영양기능연구팀) | Ji An Kim (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation)
• 허수정(식품의약품안전처 영양기능연구팀) | Soo Jung Hu (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation)
• 최윤희(식품의약품안전처 영양기능연구팀) | Yoon Hee Choi (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation)
• 오금순(식품의약품안전처 첨가물기준과) | Keum Soon Oh (Food Additives Standard division, Ministry of Food and Drug Safety) Correspondence to