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건강기능식품에서 HPLC-UVD를 이용한 자일로올리고당 시험법의 표준화 연구 KCI 등재

Studies on Xylooligosaccharide Analysis Method Standardization using HPLC-UVD in Health Functional Food

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

본 연구는 자일로올리고당의 과학적이고 체계적인 표준 화된 시험법을 마련하여 다양한 제형의 제품에 적용하고 자 하였다. 최적화된 시험법을 마련하기 위해 초음파 처 리 시간, 산 가수분해 시간 및 농도를 검토하여 전처리 방 법을 비교 평가하였으며, HPLC-UVD를 이용하여 시료 중 의 자일로올리고당을 분석하였다. 분석 시 1-phenyl-3- methyl-5-pyrazoline (PMP)으로 유도체화하고, photo diode array (PDA)가 장착된 high performance liquid chromatography (HPLC) (Nanospace SI-2)를 사용하였으며, 칼럼은 Cadenza C18 (4.6 × 250 mm, 3 μm)이었으며, 이동상은 pH를 6.0으 로 맞춘 20 mM 인산완충용액과 아세토니트릴을 78:22 비 율로 혼합하여 사용하였고, 0.5 mL/min 유속으로 254 nm 로 하여 분석하였다. 건강기능식품 등 시험법 마련 표준 절차에 관한 가이드라인에 따라 밸리데이션을 수행하고, 표준화된 시험법을 이용하여 유통 중인 건강기능식품 대 상 품목에 대해 시험법 적용 여부를 확인하였다. 표준화 된 시험법은 자일로올리고당을 함유한 건강기능식품 품질 관리에 대한 신뢰성을 더 높일 것으로 본다.

This study aimed to develop a scientifically and systematically standardized xylooligosaccharide analytical method that can be applied to products with various formulations. The analysis method was conducted using HPLC with Cadenza C18 column, involving pre-column derivatization with 1-phenyl-3-methyl-5-pyrazoline (PMP) and UV detection at 254 nm. The xylooligosaccharide content was analyzed by converting xylooligosaccharide into xylose through acid hydrolysis. The pre-treated methods were compared and evaluated by varying sonication time, acid hydrolysis time, and concentration. Optimal equipment conditions were achieved with a mobile phase consisting of 20 mM potassium phosphate buffer (pH 6)-acetonitrile (78:22, v/v) through isocratic elution at a flow rate of 0.5 mL/min (254 nm). Furthermore, we validated the advanced standardized analysis method to support the suitability of the proposed analytical procedure such as specificity, linearity, detection limits (LOD), quantitative limits (LOQ), accuracy, and precision. The standardized analysis method is now in use for monitoring relevant health-functional food products available in the market. Our results have demonstrated that the standardized analysis method is expected to enhance the reliability of quality control for healthy functional foods containing xylooligosaccharide.

목차
Materials and Methods
    시약 및 재료
    표준용액 조제
    시험용액 조제
    표준용액과 시험용액 유도체화
    국내·외 시험법 검토
    밸리데이션 방법
    기기 조건
    계산 방법
    통계 처리
Results and Discussion
    최적 분석조건 확립
    기기분석 조건 개선
    표준화 시험법 마련
    시험법 검증
    유통제품 및 시제품 적용성 검토
Acknowledgement
국문 요약
References
저자
  • 이세윤(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Se-Yun Lee (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 정희선(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Hee-Sun Jeong (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 김규헌(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Kyu-Heon Kim (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea) Corresponding author
  • 이미영(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Mi-Young Lee (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 최정호(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Jung-Ho Choi (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 안정선(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Jeong-Sun Ahn (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 권광일(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Kwang-Il Kwon (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)
  • 이혜영(식품의약품안전처 식품의약품안전평가원 영양기능연구과) | Hye-Young Lee (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety, Cheongju, Korea)