Determination of Beryllium and Selenium in Human Urine and of Selenium in Human Serum by Graphite-Furnace Atomic Absorption Spectrophotometry
Determination of Beryllium and Selenium in Human Urine and of Selenium in Human Serum by Graphite-Furnace Atomic Absorption Spectrophotometry
复制标题
DOI：
10.2116/analsci.17.527
复制
发表时间：
2001-04
影响因子：
1.6
通讯作者：
Hou-Chuan Wang;Hsien-Wen Peng;M. Kuo
中科院分区：
文献类型：
--
作者：
Hou-Chuan Wang;Hsien-Wen Peng;M. Kuo
对于人尿铍 (Be)，将每个样品 (500 μl) 用纳什试剂（含有 0.2% (v/v) 乙酰丙酮和 pH 6.0 的 2.0 M 醋酸铵缓冲液）稀释 (1+1)，然后添加 20 μl 体积的 Triton X-100 (0.4%, v/v) 水溶液。将等份（10μl）稀释的尿液混合物引入石墨比色皿中，并根据温度程序雾化。未稀释尿液样品中 Be 的方法检出限 (MDL, 3a) 为 0.37 μg/l，校准图线性高达 65.0 (μg/l)。校准图采用标准添加法绘制。测试标准参考物质 (SRM 2670) 冻干人尿样品时，准确度为 98.6-102%。尿液 Be 的精密度（相对标准偏差，RSD）为<2.3%（运行内，n = 5）和 <3.0%（运行间，n = 3） 对于人尿和血清硒 (Se)，用 HNO3（0.2%，v/v）稀释样品（1+1）以进行尿液分析或进行 (1+4) 稀释以进行血清分析。将（0.1%，v/v）加入到每200μl（1+1）稀释的尿液中（或将20μl Triton X-100加入到每500μl（1+4）稀释的血清中）样品中。将稀释的样品混合物（10μl）引入石墨比色皿中后，将相应的化学修饰剂（10μ，含有Ni^2++Pd+NH_4NO_3的HNO_3溶液）。 (0.2%, v/v)) 并将混合物雾化，未稀释样品中尿液和血清中 Se 的 MDL (3σ) 分别为 4.4 和 21.4 μ/l，校准图在 150 和 400 μg/l 范围内呈线性。通过使用 RSD 测试 SRM 2670 (NIST) 尿液标准品，尿液 Se 的准确度为 98.9–99.4%。 （批间，n = 3）在 2.9% 以内；在测试经过认证的第二代人血清（No. 29, #664）时，血清 Se 的检测结果为 97.2%，RSD（批间，n = 3）为 1.4%。该方法可以轻松、直接、准确地应用于实际样品（包括台湾黑脚病患者的 6 种尿液 Se 和 4 种血清 Se）中的 Be 和 Se 测量。
For human urine beryllium (Be), each sample (500 μl) was diluted (1+1) with Nash reagent (containing 0.2% (v/v) acetylacetone and 2.0 M ammonium acetate buffer at pH 6.0) and then a 20-μl volume of Triton X-100 (0.4%, v/v) aqueous solution was added. An aliquot (10 μl) of the diluted urine mixture was introduced into a graphite cuvette and was atomized according to a temperature program. The method detection limit (MDL, 3a) for Be was 0.37 μg/l in the undiluted urine sample and the calibration graph was linear up to 65.0 (μg/l. Calibration graphs were prepared by the standard addition method. Accuracies of 98.6- 102% were obtained when testing standard reference material (SRM 2670) freeze dried human urine samples. Precision (relative standard deviation, RSD) for urine Be was <2.3% (within-run, n = 5) and was <3.0% (between-run, n = 3). For human urine and serum selenium (Se), samples (100 μl) were diluted with HNO3 (0.2%, v/v) to make a (1+1) dilution for urine analysis or a (1+4) dilution for serum analysis. An additional aliquot (10 μl) of Triton X-100 (0.1%, v/v) was added to each 200 μl of (1+1) diluted urine (or 20 μl of the Triton X-100 was added to each 500 μl of (1+4) diluted serum) sample. After the diluted sample mixture (10 μl) was introduced into a graphite cuvette, the corresponding chemical modifier (10 μ, containing Ni^2+ + Pd + NH_4NO_3 in HNO_3 (0.2%, v/v)) was added to it and the mixture was atomized. The MDL (3σ) for Se in urine and in serum was 4.4 and 21.4 μ/l in undiluted sample, respectively, and the calibration graphs were linear up to 150 and 400 μg/l. Accuracies of urine Se were 98.9–99.4% by testing SRM 2670 (NIST) urine standards with RSD (between-run, n = 3) within 2.9%; and that of serum Se was 97.2% when testing a certified second-generation human serum (No. 29, #664) with RSD (between-run, n = 3) of 1.4%. The proposed method can be applied easily, directly, and accurately to the measurement of Be and Se in real samples (including six urine Se and four serum Se from patients of Blackfoot Disease in Taiwan).