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).

Key words: electrogenerated chemiluminescence, disposable micro-thin-layer chromatography electrode, luminol, nickel ion