高级检索

    反相高效液相色谱法测定陶瓷饰品中六价铬的溶出量

    Determination of Chromium(Ⅵ) Released from Ceramic Jewelry by Reversed-Phase HPLC

    • 摘要: 提出了柱前衍生反相高效液相色谱法测定陶瓷饰品中六价铬溶出量的方法。采用人工汗液萃取陶瓷饰品,用1,5-二苯卡巴肼与萃取液中的六价铬在酸性条件下进行衍生反应,衍生物在Waters SunFire ODS C18色谱柱上分离,以pH 2.5的10 mmol·L-1磷酸二氢钾缓冲溶液和丙酮为流动相进行梯度洗脱,于波长540 nm处进行测定。六价铬的质量浓度在5.0~200.0 μg·L-1范围内与峰面积呈线性关系,相关系数为0.999 1,检出限(3S/N)为0.037 μg·L-1。空白(实际样品)的加标回收率在97%~101%之间,测定值的相对标准偏差在1.9%~3.2%之间。

       

      Abstract: The reversed-phase high performance liquid chromatography (RP-HPLC) combined with pre-column derivatization was used to determine chromium(Ⅵ) released from ceramic jewelry. The ceramic jewelry sample was extracted by artificial sweat. Chromium(Ⅵ) in the extraction was derivatized with 1,5-diphenylcarbazide under acidic condition. The derivative was separated using Waters SunFire ODS C18 column as stationary phase and a mixture of acetone and KH2PO4 solution of 10 mmol·L-1 with pH 2.5 as mobile phase for gradient elution. Absorbance at 540 nm was measured. The linear relationship between the peak area and the mass concentration of chromium(Ⅵ) was found in the range of 5.0-200.0 μg·L-1, with correlation coefficient of 0. 999 1 and detection limit (3S/N) of 0.037 μg·L-1. Tests for recovery were made by standard addition, giving recovery rates in the range of 97%-101% and RSD (n=7) in the range of 1.9%-3.2%.

       

    /

    返回文章
    返回