高级检索

    标准加入法-微波消解-电感耦合等离子体质谱法测定人体血液中8种重金属元素和砷元素的含量

    Determination of 8 Heavy Metal Elements and Arsenic Element in Human Blood by Microwave Digestion-Inductively Coupled Plasma Mass Spectrometry with Standard Addition Method

    • 摘要: 提出了标准加入法-微波消解-电感耦合等离子体质谱法(ICP-MS)测定人体血液中铬、钴、镍、镉、锑、铊、铅、锰等8种重金属元素和砷元素含量的方法。取1 mL血液样品置于消解罐中,加入6.25 mg·L-1115In内标溶液10 μL和70%(体积分数)硝酸溶液8 mL,封闭消解罐,置于微波消解仪中消解,冷却后,置于赶酸仪中赶酸2 h,将消解液置于25 mL容量瓶中,用水清洗消解罐3次,清洗液置于同一容量瓶中,用水定容,以ICP-MS测定,使用标准加入法定量。结果表明,9种元素的质量浓度的倒数在一定范围内与所对应的响应强度与内标元素响应强度比呈线性关系,检出限(3s)为0.006 3~0.068 4 μg·L-1。回收试验中,回收率为84.4%~117%,日内(n=11)、日间(n=3)精密度试验所得测定值的相对标准偏差均小于4.0%。方法用于3份健康人体血液样品的分析,其中在人体中含量水平较低的元素,如砷、镉、锑,与文献报道较吻合。

       

      Abstract: A method for determination of 8 heavy metal elements, including chromium, cobalt, nickel, cadmium, antimony, thallium, lead, and manganese, and arsenic in human blood by microwave digestion-inductively coupled plasma mass spectrometry (ICP-MS) with standard addition method was proposed. 1 mL of blood sample was taken and placed in a digestion tank. 10 μL of 6.25 mg·L-1 115In internal standard solution and 8 mL of 70% (volume fraction) nitric acid solution were added. The digestion tank was closed and placed in a microwave digestion instrument for digestion. After cooling, the solution was placed in an acid removal device to remove acid for 2 h and the digestion solution was placed in a 25 mL-volumetric flask. The digestion tank was washed with water 3 times and the cleaning solution was placed in the same volumetric flask. The solution was made its volume with water and determined by ICP-MS, with the standard addition method for quantification. As shown by the results, linear relationships between the ratios of the corresponding response intensity to the internal standard response intensity and the reciprocal of the mass concentration of 9 elements were kept in definite ranges, with detection limits (3s) in the range of 0.006 3-0.068 4 μg·L-1. In the test for recovery, giving results in the range of 84.4%-117%. RSDs of the determined values obtained from intra-day (n=11) and inter-day (n=3) precision tests were less than 4.0%. This method was used for the analysis of 3 healthy human blood samples, the elements with lower levels in the human body, such as arsenic, cadmium, antimony, were consistent with literature reports.

       

    /

    返回文章
    返回