Machát Jirí, Kanický Viktor, Otruba Vítezslav
Laboratory of Plasma Sources for Chemical Analysis, Faculty of Science, Masaryk University Brno, Czech Republic.
Anal Bioanal Chem. 2002 Feb;372(4):576-81. doi: 10.1007/s00216-001-1188-4. Epub 2001 Dec 21.
The possibility of determining selenium in blood serum using inductively coupled plasma emission spectrometry with conventional pneumatic nebulization was studied. A high-resolution spectrometer (SBW=6 pm) with laterally viewed ICP was employed. Analysis with conventional pneumatic nebulization could overcome laborious and demanding digestion, which is necessary for hydride generation. A pressure digestion with nitric acid at 160 degrees C was sufficient to decrease the carbon content in the serum sample to 5%-10% of its original value. Spectral interference of the CN band was observed and mathematically corrected. It was found that the carbon-induced selenium line emission enhancement occurred even under ICP optimized conditions. A method of determination was developed and applied to the analysis of blood serum. True limit of detection in real samples is 0.01-0.02 mg/L and the limit of quantification (RSD 10%) is 0.03-0.07 mg/L using Se I 196.090 nm line at an integration time of 10-2 s. The method was tested by analysis of porcine blood serum and the serum reference material Seronorm MI 0181.
研究了使用具有常规气动雾化的电感耦合等离子体发射光谱法测定血清中硒的可能性。采用了配备侧向观察电感耦合等离子体的高分辨率光谱仪（SBW = 6 pm）。使用常规气动雾化进行分析可以克服氢化物发生所需的繁琐且苛刻的消解过程。在160℃下用硝酸进行压力消解足以将血清样品中的碳含量降低至其原始值的5% - 10%。观察到了CN带的光谱干扰并进行了数学校正。结果发现，即使在电感耦合等离子体优化条件下，碳也会导致硒谱线发射增强。开发了一种测定方法并应用于血清分析。在积分时间为10 - 2 s时，使用Se I 196.090 nm谱线，实际样品中的真实检测限为0.01 - 0.02 mg/L，定量限（相对标准偏差10%）为0.03 - 0.07 mg/L。通过分析猪血清和血清标准物质Seronorm MI 0181对该方法进行了测试。
