Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Error factors and uncertainty measurement for determinations of amino acid in beef bone extract

사골농축액 시료 중에 함유된 아미노산 정량분석에 대한 오차 요인 및 측정불확도 추정

  • Kim, Young-Jun (Department of Agricultural Biotechnology, Seoul National University) ;
  • Kim, Ji-Young (Department of Agro-Food safety, National Academy of Agricultural Science, Rural Development Administration) ;
  • Jung, Min-Yu (Department of Agricultural Biotechnology, Seoul National University) ;
  • Shin, Young-Jae (Department of Environmental Horticulture, Dankook University)
  • 김영준 (서울대학교 농생명공학부) ;
  • 김지영 (국립농업과학원 농산물안전성부) ;
  • 정민유 (서울대학교 농생명공학부) ;
  • 신영재 (단국대학교 환경원예학과)
  • Received : 2012.08.24
  • Accepted : 2013.03.05
  • Published : 2013.04.25
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Abstract

This study was demonstrated to estimate the measurement uncertainty of 23 multiple-component amino acids from beef bone extract by high performance liquid chromatography (HPLC). The sources of measurement uncertainty (i.e. sample weight, final volume, standard weight, purity, standard solution, calibration curve, recovery and repeatability) in associated with the analysis of amino acids were evaluated. The estimation of uncertainty obtained on the GUM (Guide to the expression of uncertainty in measurement) and EURACHEM document with mathematical calculation and statistical analysis. The content of total amino acids from beef bone extract was 36.18 g/100 g and the expanded uncertainty by multiplying coverage factor (k, 2.05~2.36) was 3.81 g/100 g at a 95% confidence level. The major contributors to the measurement uncertainty were identified in the order of recovery and repeatability (25.2%), sample pretreatment (24.5%), calibration-curve (24.0%) and weight of the reference material (10.4%). Therefore, more careful experiments are required in these steps to reduce uncertainties of amino acids analysis with a better personal proficiency improvement.

본 연구는 액체크로마토그래피를 이용하여 사골농축액 시료 중에 23종의 아미노산 정량분석 시 발생할 수 있는 측정불확도를 평가하였다. 아미노산 분석에 관여하는 측정불확도 인자로 시료량, 최종 무게, 표준품 무게, 표준품 순도, 검정곡선, 회수율 및 재현성 등을 확인하였다. GUM(Guide to the expression of uncertainty in measurement)과 EURACHEM에 근거하여 측정불확도에 대한 수학적 계산 및 통계분석을 수행하였다. 사골농축액 시료 중 총 아미노산 함량은 36.18 g/100 g이었으며, 95% 신뢰수준(k, 2.05~2.36)에서 확장불확도는 3.81 g/100 g이었다. 측정불확도의 주요 요인은 분석시의 회수율과 반복성(25.2%) > 시료전처리(24.5%) > 검정곡선(24.0%) 순으로 나타났다. 따라서 아미노산 분석 시 불확도를 줄이기 위해서는 실험자들의 주의와 개인적인 숙력도의 향상이 요구된다.

Keywords

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