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題名 | 應用離子配對高效能液相層析方法分析食鹽中碘離子含量=Determination of Iodide Ion Content in Edible Salt by Ion Pair-HPLC |
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作者 | 張俊雄; 張美華; 曾素香; 高雅敏; 闕麗卿; 施養志; | 書刊名 | 食品藥物研究年報 |
卷期 | 5 2014.12[民103.12] |
頁次 | 頁35-40 |
分類號 | 412.37 |
關鍵詞 | 食鹽; 高效液相層析儀; 碘化鉀; 碘離子; 離子對試劑; Salt; HPLC; Potassium iodide; Iodide ion; Ion-pairing reagent; |
語文 | 中文(Chinese) |
中文摘要 | 本研究建立以高效能液相層析法(high performance liquid chromatography, HPLC) 搭配移動相中含離子配對試劑(ion-pairing reagent)進行分析添加碘化鉀之食鹽中碘 含量。食鹽4 g以去離子水溶解並定容至100 mL後即進行分析,層析管柱採用C18 (4.6 mm × 15 cm, 5 μm),移動相為含1 mM氯化四正丁基銨(tetra-n-butylammonium chloride)離子之10 mM磷酸緩衝溶液與甲醇(9:1, v/v)溶液,流速為0.4 mL/min,以光 二極體陣列檢出器於波長226 nm分析。以碘化鉀為標準品,配製碘離子濃度標準 曲線範圍0.1-4 μg/mL之R2值為0.9997。於食鹽空白檢體中添加碘離子濃度為2.5、 25及100 μg/g,進行回收率及重複性(n=5)試驗,試驗結果,添加之回收率介於98.7- 100.2%,變異係數介於0.45-1.01%,定量極限為2.5 ppm。本方法應用於檢測市售添 加碘化鉀之食鹽,結果與標示(45 ppm之碘化鉀)約7.8%誤差。本方法無需經複雜的前 處理,以水溶解後即可利用HPLC進行分析,減少溶劑及試藥之使用,且分析物之滯 留時間及層析譜圖亦不受氯離子干擾影響其重複性,適合作為食鹽中碘離子含量之檢測方法。 |
英文摘要 | This study developed an ion-pair reverse-phase high performance liquid chromatography (RP-HPLC) method with direct UV detection for the determination of iodide ion content in edible salt. Commercial salt products (4 g) were directly dissolved in 100 mL deionized water prior to analysis. Separation was performed on a C18 (4.6 mm x 15 cm, 5 μm) column using a mixed water solution containing 1 mM tetran- butylammonium chloride, 10 mM phosphate buffer (pH=7) /methanol (9:1, v/v) with a flow rate of 0.4 mL/min. The system was equipped with a photodiode array detector operated at wavelength of 226 nm. The validation of the method showed high coefficient of determination (0.9997) over the concentration range of 0.1-4.0 μg/mL. The recoveries of iodide in spiked samples ranged from 98.7-100.2% (three levels, n=5) with variation coefficient between 0.45-1.01%. The limit of quantitation (LOQ) was 2.5 ppm. This method offered convenient sample preparation and analysis procedure with reduced solvent usage. Besides, there is no significant interference from chloride ion. Comparing the detected concentration of iodide with the labeled value of an edible salt sample, an average of 7.8% deviation was obtained. The result conform to TFDA’s food chemical analysis method validation specification. The developed method is suitable for quantitative determination of iodide ion content in edible salt. |
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