微波消解-原子荧光光谱法测定人血中锡

Detecting tin in human blood by microwave digestion-atomic fluorescence spectrometry

目的建立微波消解-原子荧光光谱法测定血中锡的方法。方法取1.00 mL血样加入4.00 mL质量分数为65.00%的浓硝酸和1.00 mL质量分数为68.00%的高氯酸后,用微波消解仪消化,加入质量分数为10.00%的硫脲-抗坏血酸1.00 mL,以浓度为1.5 mol/L的盐酸溶液定容至10.00 mL后,取5.00 mL样品采用原子荧光光谱法进行测定。结果方法线性范围为0.00~60.00μg/L,相关系数为0.999 5,检出限为0.01μg/L;样品加标回收率为98.80%~103.30%,批内相对标准差（RSD）为3.74%~5.26%,批间RSD为1.23%~4.45%,样品在4℃条件下至少可保存7 d。结论本方法检出限低,精密度好,灵敏度高,适用于血中锡水平的测定。

Objective To establish a method for detecting tin in human blood by microwave digestion-atomic fluorescence spectrometry. Methods The microwave digestion instrument was used to digest 1. 00 mL blood sample with 4. 00 mL concentrated nitric acid（ mass fraction 65. 00%） and 1. 00 mL perchloric acid（ mass fraction 68. 00%）. After 1. 00 mL of thiocarbamide-ascorbic acid（ mass fraction 10. 00%） was added,hydrochloric acid（ concentration 1. 5 mol / L） was added to a total constant volume of 10. 00 mL. Then 5. 00 mL of the sample was collected and detected by atomic fluorescence spectrophotometry. Results The good linear relationship was shown in the range of 0. 00-60. 00 μg / L,and the correlation coefficient was 0. 999 5. The limit of detection was 0. 01 μg / L. The average recovery rate was 98. 80%-103. 30%. The relative standard deviation（ RSD） of within-run precision was 3. 74%-5. 26%,and the RSD of betweenrun precision was 1. 23%-4. 45%. The samples can be stored for at least 7 days under the temperature of 4 ℃.Conclusion This method has the advantages of low detection limit,good precision and high sensitivity,which is suitable for the determination of tin in human blood.