Korean Journal of Food Science and Technology (한국식품과학회지)

Korean Society of Food Science and Technology (한국식품과학회)
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Simultaneous Determination of Synephrine and N-Methyltyramine in Orange Fruit and Juice from Korean Market by UPLC-FLD

UPLC-FLD를 이용한 국내 시판 오렌지 및 오렌지 주스 중 시네프린 및 n-메틸티라민 동시분석

  • Kim, Hyo Jin (Food Safety Center, Research and Development Institute, Namyang Dairy Co., Ltd.) ;
  • Kwak, Byung-Man (Food Safety Center, Research and Development Institute, Namyang Dairy Co., Ltd.) ;
  • Ahn, Jang-Hyuk (Food Safety Center, Research and Development Institute, Namyang Dairy Co., Ltd.) ;
  • Park, Jong-Su (Food Safety Center, Research and Development Institute, Namyang Dairy Co., Ltd.)
  • 김효진 (남양유업 중앙연구소 식품안전센터) ;
  • 곽병만 (남양유업 중앙연구소 식품안전센터) ;
  • 안장혁 (남양유업 중앙연구소 식품안전센터) ;
  • 박종수 (남양유업 중앙연구소 식품안전센터)
  • Received : 2013.11.15
  • Accepted : 2014.03.04
  • Published : 2014.06.30
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Abstract

An accurate and sensitive analytical method was established for the simultaneous determination of synephrine and n-methyltyramine contents by ultra-performance liquid chromatography (UPLC) with a fluorescence detector (FLD). A 70:30 (v/v) mixture of 10 mM sodium dodecyl sulfate (SDS) and acetonitrile was used as the mobile phase. The coefficient of correlation ($r^2$) was 0.9999 for both synephrine and n-methyltyramine, and their limits of detection (LOD) were 0.02 and 0.01 mg/kg, respectively. The percentage recoveries for synephrine and n-methyltyramine were 96.4% and 100.9%, respectively, from bitter orange (Citrus aurantium) samples. The synephrine and n-methyltyramine contents were 38.07-118.21 mg/kg and 0.27-0.56 mg/kg, respectively, in the orange fruit samples, while they were 14.61-120.39 mg/kg and up to 3.34 mg/kg, respectively, in the tested commercial orange juice samples. The differences in synephrine and n-methyltyramine content between orange fruit and commercial orange juice were not significant (p<0.05). These results suggest that UPLC-FLD can be applied to develop an analytical method of quality control for commercial orange juice.

본 연구에서는 UPLC를 이용하여 시네프린과 n-메틸티라민을 단시간에 동시 분석할 수 있는 새로운 방법을 개발한 후 시험법에 대한 평가를 수행하였으며, 확립된 방법으로 21종의 오렌지 및 감귤 주스와 5종의 오렌지 및 감귤에서 시네프린과 n-메틸티라민을 정량 분석을 실시하였다. UPLC를 이용하여 분석한 결과 HPLC에 비해 분석시간을 3배 이상 단축하여 15분 이내에 분석하였고, 각 성분의 감도가 월등히 높아져 UPLC로 분석 시 시간적, 경제적인 면에서 효율적으로 두 성분의 동시 분석이 가능하였다. UPLC 분석 시 검출한계는 시네프린과 n-메틸티라민이 각각 0.02 mg/L과 0.01 mg/L, 정량한계는 시네프린과 n-메틸티라민이 각각 0.06 mg/L과 0.04 mg/L로 설정되었다. 시네프린과 n-메틸티라민의 회수율은 각각 96.4%와 100.9%로 분석되었다. 확립된 분석법으로 시중에서 판매하는 오렌지 및 감귤의 과육과 과피에서 시네프린과 n-메틸티라민을 분석한 결과 모두 과육보다 과피에서 7-12배 이상 높은 함량을 나타내었다. 시판 오렌지 및 감귤 주스를 분석한 결과 시네프린 함량이 14.61-120.39 mg/kg으로 분석되었으며, n-메틸티라민은 불검출에서 3.34 mg/kg으로 분석되었다. 감귤 주스 중 과육보다 약간 높은 수준의 샘플이 있었으나 이는 천연 유래 범위 이내로 판단하였다. 따라서 본 연구에서 확립된 UPLC 분석법은 시네프린과 n-메틸티라민을 신속하고 효과적으로 동시 분석하는데 이용될 수 있을 것이며, 본 실험에 사용된 시중에 판매하고 있는 오렌지 및 감귤 주스는 자연에서 유래되는 허용 범위 내 함량을 나타내어 안전성에 문제가 없음을 알 수 있었다.

Keywords

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