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건강기능식품에서 HPLC를 이용한 4-Hydroxy-L-isoleucine 분석법 연구 KCI 등재

Development of Method for Determining 4-Hydroxy-L-isoleucine in Health Functional Foods by HPLC

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한국식품위생안전성학회지 (Journal of Food Hygiene and Safety)
한국식품위생안전성학회 (Korean Society of Food Hygiene and Safety)
초록

본 연구는 건강기능식품 호로파종자식이섬유 중 4-hydroxy- L-isoleucine에 대한 분석법을 개발하는 연구이다. 최적분석 조건을 확립하기 위해 시료 채취량, 전처리 용매 및 이동 상 용매 조건을 비교 검토하였으며, HPLC-PDA를 이용하여 시료 중의 4-hydroxy-L-isoleucine를 분석하였다. 분석 시 사용한 컬럼은 Capcell Pack UG120 C18 (Shiseido, 4.6×250 mm, 5 μm)이며, 유도체 시약으로 OPA를 선정하였다. 확립된 시험법에 대해 특이성, 직선성, 검출한계, 정량한계, 정확성, 정밀성 등의 밸리데이션을 수행하였다. 5- 100 μg/mL 농도에서 결정계수(R2) 0.999 이상으로 높은 직선성을 확인하였다. 또한, 회수율은 91.7-96.4%이었고, 정 밀성은 0.5-1.1%의 상대표준편차(%RSD)를 확인하였다. 개발된 시험법은 호로파종자추출물 중 4-hydroxy-L-isoleucine 분석을 위한 시험법으로 활용되기에 적합한 것으로 판단된다.

This study was conducted to develop a method of analysis for 4-hydroxy-L-isoleucine in the seed extract of fenugreek (Trigonella foenum graecum), a health functional food that contains dietary fiber. The analytical method for 4-hydroxy-L-isoleucine was derived with O-phthaldialdehyde reagent (OPA) and determined by HPLCPDA. The method was performed on a Capcell Pak C18 UG 120 column (4.6×250 mm, 5 μm) in isocratic elution mode using disodium phosphate and acetonitrile. The validation of the developed analytical method was conducted by evaluating several parameters; selectivity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy and repeatability. Excellent linearity (R2=0.999) was observed for 4-hydroxy-L-isoleucine in the concentration range (5- 100 μg/mL). Observed recoveries of these compounds were found to be between 91.7 and 96.4%. Precision was between 0.2 and 2.4% relative standard deviation (%RSD).

목차
ABSTRACT
Materials and Methods
    시약 및 재료
    표준용액 조제
    시험용액 조제
    최적분석조건 확립
    밸리데이션 방법
    기기조건
Results and Discussion
    최적분석조건 확립
    밸리데이션 및 적용성
    검출한계(LOD) 및 정량한계(LOQ)
국문요약
References
저자
  • 이세윤(식품의약품안전처 식품의약품안전평가원 영양기능연구팀) | Se-Yun Lee (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 정희선(식품의약품안전처 식품의약품안전평가원 영양기능연구팀) | Hee-Sun Jeong (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 허수정(식품의약품안전처 식품의약품안전평가원 영양기능연구팀) | Soo-Jung Hu (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 이혜영(식품의약품안전처 식품의약품안전평가원 영양기능연구팀) | Hye-Young Lee (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 오재명(식품의약품안전처 식품의약품안전평가원 영양기능연구팀) | Jae-Myoung Oh (Nutrition and Functional Food Research Team, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) Correspondence to