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Comparison of Extraction Methods for Determination of Vitamin K1 in Vegetables

채소류의 비타민 K1 분석을 위한 추출방법의 비교

  • Kim, Hyeongi (Brain Korea 21 Center for Bio-Resource Development & Division of Animal, Horticultural, and Food Sciences, Chungbuk National University) ;
  • Choi, Youngmin (National Academy of Agricultural Science, Rural Development Administration) ;
  • Cho, Young-Sook (National Academy of Agricultural Science, Rural Development Administration) ;
  • Sung, Jeehye (Brain Korea 21 Center for Bio-Resource Development & Division of Animal, Horticultural, and Food Sciences, Chungbuk National University) ;
  • Ham, Hyeonmi (Brain Korea 21 Center for Bio-Resource Development & Division of Animal, Horticultural, and Food Sciences, Chungbuk National University) ;
  • Lee, Junsoo (Brain Korea 21 Center for Bio-Resource Development & Division of Animal, Horticultural, and Food Sciences, Chungbuk National University)
  • 김현기 (충북대학교 식품생명공학과) ;
  • 최용민 (농촌진흥청 국립농업과학원 농식품자원부) ;
  • 조영숙 (농촌진흥청 국립농업과학원 농식품자원부) ;
  • 성지혜 (충북대학교 식품생명공학과) ;
  • 함현미 (충북대학교 식품생명공학과) ;
  • 이준수 (충북대학교 식품생명공학과)
  • Received : 2014.07.29
  • Accepted : 2014.08.28
  • Published : 2014.11.30

Abstract

The objective of this study was to compare two extraction methods for determination of vitamin K1 (phylloquinone) in vegetables. In addition, analytical method validation parameters such as accuracy, precision, limit of detection (LOD), limit of quantification (LOQ), and linearity were calculated to ensure the method's validity. Vitamin K1 was quantified by reversed-phase HPLC using post-column derivatization and fluorescence detection ($Ex{\lambda}=243nm$, $Ex{\lambda}=430nm$). Higher analytical values were observed using solvent extraction compared to those from the enzyme extraction method. The results from the method validation showed high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9994. The LOD and LOQ were 0.1335 and 0.2784 ng/injection volume ($50{\mu}L$), respectively. The inter-day precision and inter-day precision were 2.0% and 2.1%, respectively. Overall recovery was close to 100% (n=5). The phylloquinone contents ranged from 9.42 to $1,212.57{\mu}g/100g$. Our study provides reliable data on the phylloquinone contents in commonly consumed vegetables in Korea.

본 연구에서는 HPLC를 사용하여 채소류 식품군에서 비타민 K1의 분석법을 확립하고 이에 대한 분석법 검증하고자 하였다. 그 결과 본 시험법에서 표준용액의 피크유지시간과 부추 추출액의 피크유지시간이 일치하여 특이성을 확인하였다. 검량선의 상관계수($R^2$)는 0.9994 이상으로 높은 유의수준을 보여 분석에 적합함을 알 수 있었으며, 검출한계는 0.1335 ng/injection volume($50{\mu}L$)이었고 정량한계는 0.2784 ng/injection volume($50{\mu}L$)으로 설정되었다. 일내, 일간분석에서 정밀도를 나타내는 변동계수(coefficient variation, CV)는 표준용액에서 각각 1.979%, 2.107%로 나타내었고 정확성은 99.439%로 나타내어 채소류에서 비타민 K1의 분석법이 적합한 시험법임이 검증되었다. 본 분석법에 따라 채소류의 비타민 K1을 분석한 결과 식품공전의 효소를 이용한 분석법보다 더 높은 추출률을 나타내었으며 다른 물질의 간섭 없이 분석 가능하여 채소류의 비타민 K1의 검출에 응용되어 이용될 수 있을 것으로 판단된다.

Keywords

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