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利用敌草隆对三联吡啶钌电化学发光(ECL)的增敏作用,以3D石墨烯和二氧化硅固定三联吡啶钌纳米复合材料(Si O2@Ru(bpy)2+3)修饰的玻碳电极为工作电极,建立了一种直接快速检测敌草隆的电化学发光新方法。通过一步水热法合成了3D石墨烯以促进电子传递,油包水微乳液法合成Si O2@Ru(bpy)2+3以提高发光效率。在最佳实验条件下,敌草隆浓度的对数在9.08×10-11~9.08×10-7mol/L范围内与其相对发光强度呈良好的线性关系(r2=0.998 9),检出限(S/N=3)为1.18×10-12mol/L。连续测定2.00×10-8mol/L敌草隆10次,发光强度值的相对标准偏差(RSD)为4.2%,表明该方法具有良好的重复性。用该方法对青菜进行检测,回收率为99.3%~110.8%,结果满意。
The sensitizing effect of diuron on the electrochemiluminescence (ECL) of terpyridyl bipyridyl was studied. The glassy carbon modified by 3D graphene and silica-supported terpyridine ruthenium nanocomposite (Si O2 @ Ru (bpy) 2 + 3) Electrode as the working electrode, a direct and rapid detection of diuron electrochemiluminescence a new method. 3D graphene was synthesized by one-step hydrothermal method to promote electron transfer, and Si O2 @ Ru (bpy) 2 + 3 was synthesized by water-in-oil microemulsion method to improve the luminous efficiency. Under the optimal experimental conditions, the logarithm of diuron concentration showed a good linear relationship with its relative luminescence intensity (r2 = 0.998 9) in the range of 9.08 × 10-11 ~ 9.08 × 10-7 mol / L. The detection limit S / N = 3) was 1.18 × 10-12 mol / L. Continuous determination of 2.00 × 10-8mol / L diuron 10 times, the relative standard deviation of emission intensity (RSD) of 4.2%, indicating that the method has good repeatability. The method of testing vegetables, the recovery rate of 99.3% ~ 110.8%, the results are satisfactory.