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Development and Validation of Analytical Method for Decursin in Aerial Parts of Angelica gigas Nakai Extract

참당귀 지상부 추출물의 지표성분 decursin의 분석법 개발 및 검증

  • Kim, Hee-Yeon (Agriproduct Processing Experiment Station, Gangwon-do Agricultural Research and Experiment Services) ;
  • Lee, Ki-Yeon (Agriproduct Processing Experiment Station, Gangwon-do Agricultural Research and Experiment Services) ;
  • Kim, Tae-Hee (Agriproduct Processing Experiment Station, Gangwon-do Agricultural Research and Experiment Services) ;
  • Park, A-Reum (Agriproduct Processing Experiment Station, Gangwon-do Agricultural Research and Experiment Services) ;
  • Noh, Hee-Sun (Agriproduct Processing Experiment Station, Gangwon-do Agricultural Research and Experiment Services) ;
  • Kim, Si-Chang (Agriproduct Processing Experiment Station, Gangwon-do Agricultural Research and Experiment Services) ;
  • Ahn, Mun-Seob (Agriproduct Processing Experiment Station, Gangwon-do Agricultural Research and Experiment Services)
  • 김희연 (강원도농업기술원 농식품연구소) ;
  • 이기연 (강원도농업기술원 농식품연구소) ;
  • 김태희 (강원도농업기술원 농식품연구소) ;
  • 박아름 (강원도농업기술원 농식품연구소) ;
  • 노희선 (강원도농업기술원 농식품연구소) ;
  • 김시창 (강원도농업기술원 농식품연구소) ;
  • 안문섭 (강원도농업기술원 농식품연구소)
  • Received : 2018.11.29
  • Accepted : 2019.02.12
  • Published : 2019.02.28

Abstract

Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column ($3{\times}150mm$, $3{\mu}m$) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9994 and the limit of detection and limit of quantitation were $0.011{\mu}g/mL$ and $0.033{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and $10{\mu}g/mL$ were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.

본 연구에서는 건강기능성 식품 소재 개발을 목적으로 참당귀 지상부 추출물의 표준화를 위하여 decursin을 지표성분으로 선정하고 HPLC분석을 통하여 decursin의 분석법을 확립하고 유효성 검정을 수행하였다. 유효성 검정 결과, decorsin 표준용액과 참당귀 지상부 추출물의 retention time 및 spectrum이 일치하는 특이성을 확인하였다. 표준 검량선의 상관계수($R^2$)는 0.9994로 매우 우수한 직선성을 나타내었으며 정량한계(LOQ)는 $0.034{\mu}g/mL$이었고 검출한계(LOD)는 $0.011{\mu}g/mL$이었다. Decursin의 intra-day 분석에서 정확성 및 상대표준편차는 각각 96.49 ~ 104.35%, 0.53 ~ 1.10%, inter-day 분석에서 정확성 및 상대표준편차는 각각 97.23 ~ 100.14%, 0.26 ~ 1.15%인 것으로 나타나 본 시험법의 정확성 및 정밀성을 확인 할 수 있었다. 표준품 농도별 지표성분의 회수율은 92.38 ~ 104.11%의 범위였으며 분석오차 10% 이내로 측정되었다. 이는 본 연구에서 수행된 HPLC 분석법이 참당귀 지상부 추출물의 지표성분인 decursin을 분석하고 표준화하는데 적합한 시험법임을 의미한다.

Keywords

References

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