Renard Nadine E, Tompkins Thomas A
Institut Rosell, Montréal, Québec, Canada.
Biol Trace Elem Res. 2002 Aug;88(2):185-91. doi: 10.1385/BTER:88:2:185.
The selenium determination in biological materials by the classical fluorometric method (FM) is time-consuming and also hazardous, as it requires the destruction of the organic matrix samples with hot HNO3/HClO4 mixtures prior to analysis. Accordingly, commercial analytical laboratories are increasingly using faster instrumental methods; for sample digestion, avoid using HClO4. Because of these procedural changes, the results obtained by commercial laboratories may be unreliable, especially for samples containing Se in organic forms. One such "difficult" substrate is Se yeast, which contains most of its Se as selenomethionine. To establish which methods for Se analysis and sample digestion are applicable, samples of Se yeast and of selenomethionine standards were sent to laboratories employing either flame atomic absorption spectrometry (FAAS), inductively coupled plasma-mass spectrometry (ICP-MS), or hydride generation atomic absorption spectrometry (HGAAS). The results were compared with those obtained by FM and non-destructive instrumental neutron activation analysis (INAA). ICP-MS, after microwave digestion of sample with HNO3/H2O2, produced results within 5% of the expected values, as did those obtained by FM and INAA. With FAAS, acceptable results were obtained after digestion with HNO3/HCl. With HGAAS, sample digestion with HNO3/H2O2 produced values that were systematically elevated by about 10% and exhibited standard deviations of > or = 10%. Thus, current methods of sample digestion are applicable for Se yeast analysis by ICP-MS and FAAS, but not by HGAAS.
采用经典荧光法(FM)测定生物材料中的硒既耗时又危险,因为在分析之前需要用热的硝酸/高氯酸混合物破坏有机基质样品。因此,商业分析实验室越来越多地使用更快的仪器方法;对于样品消解,避免使用高氯酸。由于这些程序上的变化,商业实验室获得的结果可能不可靠,特别是对于含有有机形态硒的样品。一种这样的“难处理”底物是硒酵母,其大部分硒以硒代蛋氨酸的形式存在。为了确定哪些硒分析方法和样品消解方法适用,将硒酵母样品和硒代蛋氨酸标准品送至采用火焰原子吸收光谱法(FAAS)、电感耦合等离子体质谱法(ICP-MS)或氢化物发生原子吸收光谱法(HGAAS)的实验室。将结果与通过FM和非破坏性仪器中子活化分析(INAA)获得的结果进行比较。用硝酸/过氧化氢对样品进行微波消解后,ICP-MS得到的数据在预期值的5%以内,FM和INAA得到的结果也是如此。使用FAAS时,用硝酸/盐酸消解后得到了可接受的结果。对于HGAAS,用硝酸/过氧化氢进行样品消解得到的值系统性地高出约10%,且标准偏差大于或等于10%。因此,目前的样品消解方法适用于通过ICP-MS和FAAS分析硒酵母,但不适用于HGAAS。