Journal of Food Hygiene and Safety (한국식품위생안전성학회지)

The Korean Society of Food Hygiene and Safety (한국식품위생안전성학회)
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Development of Analytical Method for Determination of Baicalin, Eleutheroside E, and Ligustilide by LC-MS/MS in Raw Materials of Health Functional Foods

LC-MS/MS를 이용한 건강기능식품 원료 중 바이칼린, 엘레우테로사이드 E, 리구스틸라이드 동시분석법 개발

  • Keum, Eun Hee (Imported Food Analysis Division, Gyeongin Regional Food and Drug Administration, Ministry of Food and Drug Safety) ;
  • Chung, So Young (Imported Food Analysis Division, Gyeongin Regional Food and Drug Administration, Ministry of Food and Drug Safety) ;
  • Lee, Jin Hee (Imported Food Analysis Division, Gyeongin Regional Food and Drug Administration, Ministry of Food and Drug Safety) ;
  • Kim, Meehye (Imported Food Analysis Division, Gyeongin Regional Food and Drug Administration, Ministry of Food and Drug Safety)
  • 금은희 (경인지방식품의약품안전청 수입식품분석과) ;
  • 정소영 (경인지방식품의약품안전청 수입식품분석과) ;
  • 이진희 (경인지방식품의약품안전청 수입식품분석과) ;
  • 김미혜 (경인지방식품의약품안전청 수입식품분석과)
  • Received : 2017.04.11
  • Accepted : 2017.05.12
  • Published : 2017.06.30
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Abstract

Scutellaria baicalensis, Eleutherococcus senticosus, and Angelica sinensis have been used as raw materials for health functional foods. This study was conducted to develop a novel method to analyze levels of baicalin (Scutellaria baicalensis), eleutheroside E (Eleutherococcus senticosus), and ligustilide (Angelica sinensis) simultaneously in health functional foods. The methanol extracted samples were analyzed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode and the negative ion mode using multiple reaction monitoring. Standard calibration curves confirmed linearity with the correlation coefficient ($r^2$) of > 0.99 at $100-2000{\mu}g/mL$ concentration range. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $13.0{\sim}35.2{\mu}g/L$ and $39.3{\sim}106.7{\mu}g/L$, respectively. The recovery results ranged between 91.4~109.9% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high accuracy and acceptable precision. The new method would be an effective tool to analyze baicalin, eleutheroside E, and ligustilide simultaneously in raw materials of health functional foods.

본 연구는 건강기능식품 중 baicalin, eleutheroside E, ligustilide를 효과적으로 분석할 수 있는 방법을 확립하기 위하여 수행되었다. 이에 LC-MS/MS를 이용하여 신속하고 효율적으로 동시분석할 수 있는 시험법을 확립하였으며, 확립된 시험법에 대해 특이성, 검출한계, 정량한계, 정확도, 정밀도에 대한 검증을 통하여 유효성을 확인하고자 하였다. 표준용액을 이용하여 검량선을 작성한 결과 $r^2$ > 0.99 이상의 직선성을 확인하였고, baicalin, eleutheroside E, ligustilide에 대한 정량한계는 각각 $39.3{\mu}g/L$, $106.7{\mu}g/L$, $76.1{\mu}g/L$이었으며, 검출한계는 각각 $13.0{\mu}g/L$, $35.2{\mu}g/L$, $25.1{\mu}g/L$이었다. 또한 평균 회수율은 각 성분에 대해 108.0~109.9%, 99.8~101.3%, 91.4~97.2%로 나타났으며, 반복정밀도는 상대표준편차 5%이하, 실험실간 재현성은 9%이하로 나타나 정확성, 재현성이 우수하였으며 이는 AOAC 가이드라인에서 제시한 기준에 모두 적합한 수준이었다. 따라서 개발된 분석법은 향후 건강기능식품 중 baicalin, eleutheroside E, ligustilide를 동시분석하는데 효과적으로 활용할 수 있을 것으로 판단된다.

Keywords

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