Group of Analytical Chemistry, Automation, and Environment, Dep. Chemistry, Universitat de les Illes Balears, 07122 Palma de Mallorca, Spain.
Talanta. 2010 Apr 15;81(1-2):572-7. doi: 10.1016/j.talanta.2009.12.045. Epub 2010 Jan 4.
In the present work, a solid phase extraction (SPE) is hyphenated with an automatic MSFIA system to improve the selenite determination based on the reaction of selenite with aromatic o-diamines (such as 2,3-diaminonaphthalene (DAN)) to form the piazselenol complex. This reaction is greatly influenced by acid concentration, temperature, the time needed for colour development, and presence of foreign ions. For these reasons a thermostatic bath, glycine, and Na(2)-EDTA are used as heater, buffer, and masking agent, respectively. The principle of the determination is based on the sorption of the piazselenol onto a C(18) membrane disk, followed by its elution by acetonitrile. The piazselenol can then be detected by absorptiometry or fluorometry, both detection techniques being tested in our system. The best detection limit (1.7 microg L(-1)) and RSD (3.04%) are obtained by absorptiometry at 380 nm. Environmental samples were spiked and analyzed, with recoveries close to 100%.
在本工作中，采用固相萃取（SPE）与自动 MSFIA 系统联用，以提高亚硒酸盐的测定。亚硒酸盐与芳香族邻二胺（如 2,3-二氨基萘（DAN））反应形成吡唑硒醇络合物，基于此反应进行测定。该反应受到酸浓度、温度、显色时间以及共存离子的影响较大。因此，使用恒温水浴、甘氨酸和 Na(2)-EDTA 分别作为加热器、缓冲液和掩蔽剂。测定原理基于将吡唑硒醇吸附到 C(18)膜盘上，然后用乙腈洗脱。吡唑硒醇随后可以通过吸光光度法或荧光光度法进行检测，我们的系统中测试了这两种检测技术。在 380nm 处，吸光光度法的最佳检测限（1.7μg L(-1)）和 RSD（3.04%）。对环境样品进行了加标分析，回收率接近 100%。
