油脂食品中維生素E檢驗方法之確效及不確定度之評估

The Certification and Analysis Uncertainties of the HPLC Method for Assay of Vitamin E in Edible Fats and Oils

10.6946/ASRNL.200309.0168

蔡佳芬(Chia-Fen Tsai)；陳啟民(Chi-Min Chen)；潘志寬(Jyh-Quan Pan)

油脂食品 ； 維生素E ； 確效 ； 高效液相層析法 ； 不確定度 ； edible fats and oils ； vitamin E ； certification ； HPLC ； uncertainty

藥物食品檢驗局調查研究年報

21號（2003 / 09 / 01）

168 - 180

繁體中文

建立以高效液相層析法分析油脂食品中維生素E（dl-α-tocopherol及dl-α-tocopheryl acetate）含量之檢驗方法，並進行方法之確效。油脂食品以正己烷適量稀釋，經微孔過濾膜過濾後，以高效液相層析分析，其分析條件：液相層析管柱：C18(4.6×300 mm)，移動相：甲醇，流速：1.0 mL/min，檢出器：紫外光波長280nm。方法之確效包括添加回收試驗、空白試驗、最低檢出限量、查核物質之檢驗、重複性試驗等。添加濃度20~1000 ppm時之添加回收率於dl-α-tocopherol為94.5~111.4%，變異係數為0.2~2.4%；dl-α-tocopheryl acetate為91.3~118.8%，變異係數為0.2~1.0%。空白試驗檢出值均為0。dl-α-tocopherol及dl-α-tocopheryl acetate之最低檢出限量均為10 ppm。以查核物質進行10次重複試驗之平均回收率為99.3%，SD為3.003。而在信賴區間95%之量測不確定度均為量測值之4.76%。

This study was aimed at establishing and certifying the HPLC method for assay of vitamin E in edible fats and oils. The sample was diluted with n-hexane and analyzed by HPLC. HPLC conditions were as follows, column: C18 (4.6×300 mm); mobile phase: methanol; flow rate：1 mL/min; detecting wavelength: UV 280 nm. The tests included recovery, blank study, detection limit, check sample test and repetition study. The recovery rates were 94.5-111.4% for the spiked concentrations at 20-1000 ppm of dl-α-tocopherol, and 91.3-118.8% for the spiked concentrations at 20-1000 ppm of dl-α-tocopheryl acetate, the variation coefficients were 0.2-2.4% and 0.2-1.0%. The blank test was 0. The detection limit of the method was 10 ppm for dl-α-tocopherol and dl-α-tocopheryl acetate in edible fats and oils. The average recovery rate of tenth tests for check sample was 99.3%, SD was 3.003. The expanded uncertainties were 4.76%, which were obtained by multiplying the combined standard uncertainties by a coverage factor of 2.