摘要
通过电聚合和电沉积方法首次制得聚(三聚氰胺)和金纳米粒共修饰的电极(PMel/Au/GCE),并对修饰电极进行交流阻抗电化学分析。采用循环伏安法研究了芦丁在修饰电极上的电化学行为,发现其氧化峰电流和还原峰电流较裸玻碳电极(GCE)以及聚(三聚氰胺)修饰的电极(PMel/GCE)明显增强,提高了检测的灵敏度。对溶液的pH值、金纳米粒子电沉积时间、三聚氰胺电聚合时间和扫描速率等实验条件进行了优化。采用示差脉冲伏安法对芦丁进行定量分析,芦丁浓度分别在7.8×10-9~1.2×10-6mol/L和1.2×10-6~1.5×10-5mol/L范围内与峰电流呈线性,其相关系数(r2)分别为0.997和0.993,检出限(S/N=3)为5.5×10-9mol/L。将该电极用于市售芦丁片检测,回收率为96.4%~101.8%。
An electrode modified by gold nanoparticles (AuNPs) and polymerized film of melamine (PMel) (PMel/Au/GCE) was fabricated. Electrochemical impedance spectroscopy (EIS) was used for analyzing the modified electrode. The electrochemical behavior of rutin was investigated by cyclic vohammetry (CV) , and a couple of sensitive and reversible redox peaks were obtained with an oxida- tion peak at 0.422 V and a reduction peak at 0. 374 V. It was found that the oxidation peak current (Ipa) and the reduetive peak(Ipc) current at PMel/Au/GCE were obviously larger than those at bare glassy carbon electrode (GCE) and the electrode modified by polymerized film of melamine (PMel/ GCE), which indicated that the sensitivity for detection of rutin was improved. Experimental parameters, including pH value of buffer solution, electro-deposited time of AuNPs, electro-polymerized time of PMel and scan rate were optimized. The differential pulse vohammetry (DPV) was used for the quantitative analysis on rutin. Good linear relationships between current intensities and rutin concentrations were obtained in the ranges of 7.8 x 10-9 - 1.2 x 10-6 mol/L and 1.2 x 10-6 - 1.5 x 10-5mol/L, with correlation coefficients(r2) of 0.997 and 0.993, respectively. The detection limit ( S/N = 3) was 5.5 x 10 -9 mol/L. The modified electrode was applied in the determination of rutin in rutin tablets with recoveries of 96.4% - 101.8%.
出处
《分析测试学报》
CAS
CSCD
北大核心
2014年第9期1019-1025,共7页
Journal of Instrumental Analysis
基金
国家自然科学基金(51173128)
国家科技部计划项目(2013AA102204
2012YQ090194-5)
北洋青年学者计划项目(2012)