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林立, 姚继军, 杨仁康, 孙继红. 悬浮进样-石墨炉原子吸收光谱法直接测定化妆品中的铅[J]. 岩矿测试, 2013, 32(4): 644-648.
引用本文: 林立, 姚继军, 杨仁康, 孙继红. 悬浮进样-石墨炉原子吸收光谱法直接测定化妆品中的铅[J]. 岩矿测试, 2013, 32(4): 644-648.
Li LIN, Ji-jun YAO, Ren-kang YANG, Ji-hong SUN. Direct Determination of Pb in Cosmetics by Graphite Furnace Atomic Absorption Spectrometry with Suspension Sampling[J]. Rock and Mineral Analysis, 2013, 32(4): 644-648.
Citation: Li LIN, Ji-jun YAO, Ren-kang YANG, Ji-hong SUN. Direct Determination of Pb in Cosmetics by Graphite Furnace Atomic Absorption Spectrometry with Suspension Sampling[J]. Rock and Mineral Analysis, 2013, 32(4): 644-648.

悬浮进样-石墨炉原子吸收光谱法直接测定化妆品中的铅

Direct Determination of Pb in Cosmetics by Graphite Furnace Atomic Absorption Spectrometry with Suspension Sampling

  • 摘要: 化妆品样品中金属元素的分析一直存在着样品消解过程繁琐、易爆沸等问题,前处理过程不易控制,试剂消耗大,同时也易带入铅的空白污染;且现有化妆品中铅的含量远远低于国家标准规定的限量要求( < 40 mg/kg),火焰原子吸收光谱法无法准确检测。本文建立了悬浮进样-石墨炉原子吸收光谱仪直接测定化妆品中铅的方法。样品无需消解,采用0.2%硝酸和0.1%曲拉通X-100对样品进行悬浮后直接导入石墨炉原子吸收光谱仪进行测定。在石墨炉灰化过程中不使用常规的高纯氩气,而是使用具有氧化能力的干燥压缩空气,消除了单次分析超过50个样品时产生的碳残留,保证长期分析的稳定性;采用硝酸钯作为基体改进剂,钯能与铅形成铅钯金属互化物,非常稳定,显著提高了原子化温度;采用标准加入法消除基体干扰,保证分析数据的准确性。方法检出限为0.003 mg/kg,加标回收率为91.6%~106.8%,精密度为1.5%~2.1%(n=6)。该方法应用于分析国家标准物质GBW(E) 090028(霜铅)和GBW(E) 090027(粉铅),铅的测定值与标准值吻合;与国家标准方法的测定结果进行比较,无显著性差异。本方法的检出限低,可以满足化妆品中痕量铅的检测需求。

     

    Abstract: There have been many difficulties surrounding cumbersome digestion processes and explosive boiling when attempting to detect metal elements in cosmetics. It is difficult to control the pretreatment process and it is necessary to use a lot of reagents, which easily leads to the high reagent blank. Content of lead (Pb) in cosmetics is far below the national limits (≤40 mg/kg), which cannot accurately be determined by flame atomic absorption spectrometric. In this paper a method is described for direct determination of Pb in cosmetics by Graphite Furnace Atomic Absorption Spectrometry with suspension sampling. Sample digestion was not required as the cosmetics samples to be determined were directly placed into the Graphite Furnace Atomic Absorption Spectrometer after suspension by 0.2% nitric acid and 0.1% Triton X-100. The instrument conditions were optimized and high pure argon was added to the drying compressed air in the graphite furnace ashing process, in order to eliminate the carbon residue when the number of samples was over 50, and to ensure the stability for long-term analysis. The matrix modifier was palladium nitrate. Palladium and Pb can form a stable palladium Pb metal compound, and significantly improve the atomic temperature. Standard addition method was conducted to eliminate the matrix interference. The detection limit of this method was 0.003 mg/kg.The recovery of Pb was in the range of 91.6%-106.8%, precision was in the range of 1.5%-2.1% (n=6). National standard reference materials GBW (E) 090028 (cream) and GBW(E) 090027 (powder) were determined by using this method and the results were consistent with the standard value. Compared with the results using the national standard method for detection, the results showed no significant difference. This method has low detection limit, can meet the testing requirements of trace Pb in cosmetics.

     

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