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題名 | 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 |
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作者姓名(中文) | 蔡佳芬; 陳啟民; 潘志寬; | 書刊名 | 藥物食品檢驗局調查研究年報 |
卷期 | 21 2003.08[民92.08] |
頁次 | 頁168-180 |
分類號 | 412.37 |
關鍵詞 | 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; |
語文 | 中文(Chinese) |
中文摘要 | 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280 nm。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﹪。 |
英文摘要 | 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. |
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