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    高效液相色谱-电感耦合等离子体质谱法同时测定烟用接装纸中三价铬与六价铬的含量

    Simultaneous Determination of Cr(Ⅲ) and Cr(Ⅵ) in Cigarette Tipping Paper by HPLC-ICP-MS

    • 摘要: 烟用接装纸样品1.000 g置于50 mmol·L-1氢氧化钠溶液15 mL中回旋振荡提取2 h,过滤。取其提取液0.5 mL,用0.1 mol·L-1盐酸溶液中和至pH 7.0后,加入0.1 mol·L-1 Na2-EDTA溶液5 mL,在80℃条件下反应20 min。所得溶液进行色谱分离,用Dionex AS19色谱柱为固定相,用pH 7.0的0.15 mol·L-1硝酸铵溶液作为流动相。在质谱分析中,用氦气作为碰撞气,可减小35Cl16O1H+40Ar12C+52Cr+的质谱干扰。结果表明:Cr(Ⅲ)和Cr(Ⅵ)的线性范围依次为20.0~1 000 μg·L-1,0.20~10.0 μg·L-1,检出限(3s)分别为4.81,0.63 μg·kg-1。在3个浓度水平上进行加标回收试验,测得两者的回收率依次在95.2%~104%和80.0%~116%之间,测定值的相对标准偏差(n=7)依次在2.5%~3.1%和2.6%~3.6%之间。

       

      Abstract: Sample of cigarette tipping paper 1.000 g was extracted with 15 mL of 50 mmol·L-1 NaOH solution by vortical oscillation for 2 h and then filtered. The extract (0.5 mL) was separated and neutralized with 0.1 mol·L-1 HCl solution to pH 7.0. After addition of 5 mL of 0.1 mol·L-1 Na2-EDTA solution, the extract was kept at 80℃ for 20 min, and the solution was separated chromatographically by using Dionex AS19 column as the stationary phase, and 0.15 mol·L-1 NH4NO3 solution (pH 7.0) as the mobile phase. In ICP-MS analysis, helium was used as the collision gas so as to reduce the MS interference of 35Cl16O1H+ and 40Ar12C+ to 52Cr+. Linearity ranges were found 20.0-1 000 μg·L-1 for Cr(Ⅲ) and 0.20-10.0 μg·L-1 for Cr(Ⅵ) with values of detection limits (3s) of 4.81, 0.63 μg·kg-1 respectively. Test for recovery was made by standard addition method at 3 concentration levels, giving results in the range of 95.2%-104% for Cr(Ⅲ), and 80.0%-116% for Cr(Ⅵ), with RSDs (n=7) in the range of 2.5%-3.1% for Cr(Ⅲ), 2.6%-3.6% for Cr(Ⅵ).

       

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