Naujalis Evaldas, Padarauskas Audrius
Department of Analytical and Environmental Chemistry, UNESCO Trace Element Institute Satellite Center, Vilnius University, Naugarduko 24, LT-2006 Vilnius, Lithuania.
J Chromatogr A. 2002 Nov 15;977(1):135-42. doi: 10.1016/s0021-9673(02)01350-x.
A new capillary electrophoretic (CE) method was developed for the selective and sensitive determination of common metal ions. The proposed method is based on conventional CE separation of metal cations followed by complete complexation of separated analytes with 1,10-phenanthroline using the zone-passing technique. This approach combines both partial and complete complexation modes and, thus, enables rapid, selective, efficient separation together with sensitive direct UV detection of metal species. The optimal conditions for the separation and derivatization reaction were established by varying type of electrolyte, electrolyte pH, introduction time and concentration of 1,10-phenanthroline. The optimized separations were carried out in 50 mmol l(-1) glycolic acid electrolyte (pH 6.0 with imidazole) using direct UV detection at 254 nm. Five common metal cations (Fe2+, Co2+, Ni2+, Cu2+ and Zn2+) were separated in less than 4 min. The proposed system was applied to the determination of Fe(II) and Zn(II) in snow samples. The recovery tests established for snow samples were within the range 100+/-12%.
开发了一种用于选择性和灵敏测定常见金属离子的新型毛细管电泳(CE)方法。所提出的方法基于金属阳离子的常规CE分离,然后使用区带通过技术使分离出的分析物与1,10 - 菲咯啉完全络合。这种方法结合了部分络合和完全络合模式,因此能够实现快速、选择性、高效的分离以及对金属物种的灵敏直接紫外检测。通过改变电解质类型、电解质pH值、进样时间和1,10 - 菲咯啉浓度,确定了分离和衍生化反应的最佳条件。优化后的分离在50 mmol l(-1)乙醇酸电解质(pH 6.0,含咪唑)中进行,使用254 nm的直接紫外检测。五种常见金属阳离子(Fe2 +、Co2 +、Ni2 +、Cu2 +和Zn2 +)在不到4分钟内即可分离。所提出的系统应用于雪样中Fe(II)和Zn(II)的测定。对雪样进行的回收率测试在100±12%的范围内。