基于一次性薄层色谱电极高选择电化学发光分析法测定Ni(II)的研究

基于一种新的电极制作方法, 研制了具有薄层色谱分离功能的一次性薄层色谱电极. 结合该电极的分离、保留分析物于电极表面一定空间区域的色谱分离能力与电极表面电化学发光信号的空间分辨能力, 实现了分析物的高效分离与原位高灵敏度电化学发光(ECL)检测, 建立了电化学发光分析方法与薄层色谱分离方法联用的新技术. 并以Ni^2＋离子为代表探讨了这一方法的可行性和分析特性. 在最佳的实验条件下, 该方法测定Ni^2＋离子的线性范围为5.0× 10^－9～5.0×10^－6 g/mL, 检出限为1.5×10^－9 g/mL, 相对标准偏差为2.8% (c＝1.0×10^－6 g/mL, n＝11).

Highly Selective Electrogenerated Chemiluminescence Method for Determination of Ni(II) with the Disposable Micro-Thin-Layer Chromatography Electrode

Based on a new method of electrode preparation, a novel disposable micro-thin-layer chromatography electrode with the separating function of thin-layer chromatography (TLC) was designed. Combined the ability of separating, retaining the analyte in a certain space of the electrode with the high spatial-resolved ability of electrogenerated chemiluminescence (ECL) signal on the surface of electrode, this method attained highly effective and in situ separation, highly sensitive electrogenerated chemiluminescence detection to the analyte, and a novel method is presented for the coupling of thin-layer chromatography with the ECL. The feasibility and analytical performance of this method was investigated by choosing Ni^2＋ as the analyte. Under the optimal experiment conditions, the linear range of the proposed ECL method for Ni^2＋was 5.0×10^－9 to 5.0×10^－6 g/mL with a 1.5×10^－9 g/mL detection limit, and the relative standard deviation was 2.8% (c＝1.0×10^－6 g/mL, n＝11).