摘要
目的建立尿中锡的原子荧光分光光度测定方法。方法取2.50 mL尿样加入1.50 mL浓硝酸后,用石墨消解仪消化,以体积分数为4.00%的盐酸溶液定容至10.00 mL,加入质量浓度为100 g/L的硫脲-抗坏血酸2.50 mL,以体积分数为4.00%的盐酸溶液定容至25.00 mL(相当于稀释尿样10倍)后,取1.00 mL样品采用原子荧光光度法进行测定。结果尿中锡在质量浓度为4.00~200.00μg/L范围内线性关系良好,相关系数为0.999 5;方法检出限为0.20μg/L,加标回收率为100.20%~100.84%,批内相对标准偏差(RSD)为0.11%~2.01%,批间RSD为1.37%~5.58%;样品在4℃条件下可保存7 d。结论本方法灵敏度高,准确性好,操作简便,适用于人尿中锡的日常监测。
Objective To establish a method for determination of urinary tin by atomic fluorescence spectrophotometry.Methods The graphite digestion instrument was used to digest 2. 50 m L urinary sample with 1. 50 m L concentrated nitric acid,hydrochloric acid( volume fraction 4. 00%) was added to a total constant volume of 10. 00 m L. After 2. 50 m L of thiocarbamide-ascorbic acid( mass concentration 100 g / L) was added,hydrochloric acid( volume fraction 4. 00%) was added to a total constant volume of 25. 00 m L( equivalent to urinary sample was diluted 10 times),1. 00 m L of the sample was collected and detected by atomic fluorescence spectrophotometry. Results The good linear relationship was shown in the range of 4. 00-200. 00 μg / L with a correlation coefficient of 0. 999 5. The limit of detection was 0. 20 μg / L. The recovery rates ranged from 100. 20% to 100. 84%. The within-run relative standard deviation( RSD) and between-run RSD were 0. 11%-2. 01% and 1. 37%-5. 58%,respectively. The samples can be stored for 7 days under the temperature of4 ℃. Conclusion This method has the advantages of high sensitivity,precision and convenient operation,which is suitable for the daily determination of urinary tin in human.
出处
《中国职业医学》
CAS
北大核心
2016年第3期354-357,共4页
China Occupational Medicine
基金
广州市民生科技重大项目(2014Y2-00067)
广东省"十二五"医学重点专科
广州市医学重点学科建设项目
广州市职业环境与健康效应实验室建设项目(2014SY000020)
广州市"121人才梯队工程"后备人才项目
关键词
尿锡
原子荧光光度法
石墨消解
Urinary tin
Atom fluorescence spectrophotometry
Graphite digestion