微波消解-电感耦合等离子体质谱法测定麻黄中的铜、锰、锌、镍

Determination of Copper, Manganese, Zinc and Nickel in Herbal Ephedrae by ICP-MS with Microwave Digestion

  • 摘要: 为了准确测定麻黄中的微量元素,用微波消解法对样品进行前处理,以锗(72Ge)为内标,建立了电感耦合等离子体质谱测定麻黄中4种微量元素铜、锰、锌、镍的方法。实验测得麻黄中铜、锰、锌、镍的含量分别为2.7、33.2、1.1和4.23mg/kg。结果显示,各元素线性范围为0~100μg/L,方法的检出限为0.09~0.37 μg/L,线性相关系数r在0.9996~0.999 9之间。利用精密度考查了方法的重现性,各元素的相对标准偏差(n=6)在1.26%~6.01%之间;为了考查方法的准确性,对每个元素分别测定3个不同添加浓度下的加标回收率,平均加标回收率在87.1%~113.3%之间。用该方法测定了国家一级标准物质黄芪(GBW 10028)中上述4种元素含量,测定结果与标实值一致。

     

    Abstract: The contents of traceelements of copper, manganese, zinc and nickel in Chinese traditional medicineHerbal Ephedrae were determined by inductively coupled plasma mass spectrometry(ICP-MS) with microwave digestion. The ion source and the mass spectrometeroperation parameters were optimized. The metal concentrations in HerbalEphedrae are 2.7,33.2,1.1 and 4.23 mg/kg for Cu, Mn, Zn and Ni,respectively. During the measurement, 72Ge was used as the internalstandard element. The detection limits (S/N=3) of the method are 0.09—0.37 μg/L.The results show that the linearities of the four elements are 0—100 μg/L,and the correlation coefficient are 0.999 6—0.999 9. The relative standard derivations (RSDs) are1.26%—6.01%. The averagerecoveries in a sample at three levels are in the range of 87.1%—113.3%. The results of determining the four elementsin the certified reference materials of GBW10028 are all within the ranges ofstandard values.

     

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