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使用水/油反相微乳法合成包埋联吡啶钌(Ru(bpy)32+)的纳米硅球(RuSiNPs),利用Nafion材料固定RuSiNPs于玻碳电极上,构筑了RuSiNPs/Nafion复合膜修饰传感电极,进行了醇类的电致化学发光-高效液相色谱(ECL-HPLC)分离检测.利用循环伏安等方法考察了RuSiNPs/Nafion复合膜电极的电化学和ECL行为,结果表明包埋在硅球里的Ru(bpy)32+较好地保持了原有的光学和电化学性质.研究了实验条件对其ECL的影响,通过HPLC条件的优化建立了利用RuSiNPs/Nafion固态ECL进行醇类样品的分离检测方法,所提出方法对甲醇、乙醇、丙醇和丁醇的检测下限分别为6.7×10-5,8.2×10-5,3.9×10-4和4.2×10-4mol/L.方法被初步应用于一些啤酒样品中醇的检测.
Nanosilica balls (RuSiNPs) embedded with Ru (bpy) 32+ were synthesized by water / oil reverse microemulsion method. The RuSiNPs / Nafion composite films were modified by immobilizing RuSiNPs on glassy carbon electrode by Nafion. (ECL-HPLC), the electrochemical and ECL behaviors of RuSiNPs / Nafion composite membrane electrode were investigated by cyclic voltammetry and the results showed that the Ru (bpy) 32+ embedded in the silica ball retains its original optical and electrochemical properties well.The effect of experimental conditions on its ECL has been investigated by using the optimized conditions of the HPLC to establish a solid state ECL using RuSiNPs / Nafion The method for the separation and detection of alcoholic samples showed that the detection limits of the proposed methods for methanol, ethanol, propanol and butanol were respectively 6.7 × 10-5, 8.2 × 10-5, 3.9 × 10-4 and 4.2 × 10-4mol / L The method was initially applied to the determination of alcohol in some beer samples.