Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Studies on Xylooligosaccharide Analysis Method Standardization using HPLC-UVD in Health Functional Food

건강기능식품에서 HPLC-UVD를 이용한 자일로올리고당 시험법의 표준화 연구

  • Se-Yun Lee (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Hee-Sun Jeong (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kyu-Heon Kim (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Mi-Young Lee (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Jung-Ho Choi (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Jeong-Sun Ahn (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Kwang-Il Kwon (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety) ;
  • Hye-Young Lee (Nutrition and Functional Food Research Division, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
  • 이세윤 (식품의약품안전처 식품의약품안전평가원 영양기능연구과) ;
  • 정희선 (식품의약품안전처 식품의약품안전평가원 영양기능연구과) ;
  • 김규헌 (식품의약품안전처 식품의약품안전평가원 영양기능연구과) ;
  • 이미영 (식품의약품안전처 식품의약품안전평가원 영양기능연구과) ;
  • 최정호 (식품의약품안전처 식품의약품안전평가원 영양기능연구과) ;
  • 안정선 (식품의약품안전처 식품의약품안전평가원 영양기능연구과) ;
  • 권광일 (식품의약품안전처 식품의약품안전평가원 영양기능연구과) ;
  • 이혜영 (식품의약품안전처 식품의약품안전평가원 영양기능연구과)
  • Received : 2023.08.09
  • Accepted : 2023.10.30
  • Published : 2024.04.30
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Abstract

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.

본 연구는 자일로올리고당의 과학적이고 체계적인 표준화된 시험법을 마련하여 다양한 제형의 제품에 적용하고자 하였다. 최적화된 시험법을 마련하기 위해 초음파 처리 시간, 산 가수분해 시간 및 농도를 검토하여 전처리 방법을 비교 평가하였으며, HPLC-UVD를 이용하여 시료 중의 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 ㎛)이었으며, 이동상은 pH를 6.0으로 맞춘 20 mM 인산완충용액과 아세토니트릴을 78:22 비율로 혼합하여 사용하였고, 0.5 mL/min 유속으로 254 nm로 하여 분석하였다. 건강기능식품 등 시험법 마련 표준절차에 관한 가이드라인에 따라 밸리데이션을 수행하고, 표준화된 시험법을 이용하여 유통 중인 건강기능식품 대상 품목에 대해 시험법 적용 여부를 확인하였다. 표준화된 시험법은 자일로올리고당을 함유한 건강기능식품 품질관리에 대한 신뢰성을 더 높일 것으로 본다.

Keywords

Acknowledgement

본 연구는 2021년도 식품의약품안전처 연구개발사업의 연구비지원(21161미래식044)에 의해 수행되었으며, 이에 감사드립니다.

References

  1. Ministry of Food and Drug Safety (MFDS), 2023. Health functional food code (2023-50), Cheongju, Korea.
  2. Gupta, P., Agarwal, P., Hegde, P.A., A review on xylooligosaccharides. Int. Res. J. Pharm., 3, 71-74 (2012).
  3. Kyung, M.O., Choe, H.S., Jung, S.W., Lee, K.S., Jo, S.E., Seo, S.W., Choe, K.B., Yang, C.K., Yoo, S.H., Kim, Y.R., Effect of xylooligosaccharide-sugar mixture on glycemic index (GI) and blood glucose response in healthy adults. J. Nutr. Health, 47, 229-235 (2014). https://doi.org/10.4163/jnh.2014.47.4.229
  4. Nam, H.K., Kyung, M.O., Seo, S.W., Jung, S.W., Chang, M.J., Effect of different levels of xylooligosaccharide in sugar on glycemic index and blood glucose respone in healthy adults. J. Nutr. Health, 48, 398-406 (2015). https://doi.org/10.4163/jnh.2015.48.5.398
  5. Carvalho, A., Neto, P., Silva, D., Pastore, G., Xylo-oligosaccharides from lignocellulosic materials: chemical structure, health benefits and production by chemical and enzymatic hydrolysis. Food Res. Int., 51, 75-85 (2013). https://doi.org/10.1016/j.foodres.2012.11.021
  6. Singh, R., Banerjee, J., Arora, A., Prebiotic potential of oligosaccharides: a focus on xylan derived oligosaccharides. Bioact. Carbohydr. Diet. Fibre., 5, 19-30 (2015). https://doi.org/10.1016/j.bcdf.2014.11.003
  7. Mandelli, F., Brenelli, L.B., Almeida, R.F., Goldbeck, R., Wolf, L.D., Hoffmam, Z.B., Ruller, R., Rocha, G.J.M., Mercadante, A.Z., Squina, F.M., Simultaneous production of xylooligosaccharides and antioxidant compounds from sugarcane bagasse via enzymatic hydrolysis. Ind. Crops Prod., 52, 770-775 (2014). https://doi.org/10.1016/j.indcrop.2013.12.005
  8. George, W.L. Jr., 2016. Appendix K: guidelines for dietary supplements and botanicals. Official methods of analysis of AOAC INTERNATIONAL, 20th ed, Rockville, MD, USA, pp. 1-32.
  9. Ministry of Food and Drug Safety (MFDS), 2009. Certificate of functional ingredient: xylooligosaccharide powder (No. 2009-80), Cheongju, Korea.
  10. Ministry of Food and Drug Safety (MFDS), 2009. Certificate of functional ingredient: xylooligosaccharide liquid (No. 2009-81), Cheongju, Korea.
  11. George, W.L. Jr., 2016. Arabinose, galactose, and xylose and other sugar in sugars and syrups. Official methods of analysis of AOAC INTERNATIONAL, 20th ed, Rockville, MD, USA, pp. 44.1.28.
  12. United States Pharmacopeial Convention, (2023, August 3). Xylose. Retrieved from https://online.uspnf.com/uspnf/document/1_GUID-68BDA798-EB8A-400C-97CD-A1F359F9D805_5_en-US.
  13. Yohei, Y., Hideki, K., Yasunori, K., Wataru, S., Yuya, K., Hajime, Y., Takao, O., Enzymatic production of xylooligosaccharides from red alga dulse (Palmaria sp.) wasted in Japan. Process Biochem., 82, 117-122 (2019). https://doi.org/10.1016/j.procbio.2019.03.030
  14. Chuannan, L., Jingjing, C., Hailong, L., Jian, L., Lihui, G., Bin Z., Minnan, L., Improvement in xylooligosaccharides production by knockout of the β-xyl1 gene in Trichoderma orientalis EU7-22. Biotech, 3, 8-26 (2018).
  15. Morgan, N.K., Wallace, A., Bedford, M.R., Choct, M., Efficiency of xylanases from families 10 and 11 in production of xylo-oligosaccharides from wheat arabinoxylans. Carbohydr. Polym., 167, 290-296 (2017). https://doi.org/10.1016/j.carbpol.2017.03.063
  16. Pu, J., Zhao, X., Wang, Q., Wang, Y., Zhou, H., Development and validation of a HPLC method for determination of degree of polymerization of xylo-oligosaccharides. Food Chem., 213, 654-659 (2016).