基于羧基化多壁碳纳米管修饰玻碳电极快速检测氨基脲的研究

基于羧基化多壁碳纳米管修饰的玻碳电极(CMWCNTs/GCE),构建了一种灵敏检测氨基脲(SEM)的电化学传感器.采用傅里叶变换红外光谱、透射电子显微镜、电化学阻抗谱对修饰材料进行表征.结果表明,羧基化的多壁碳纳米管出现羧基碳氧双键的红外特征峰,管径明显减小,长度变短,电化学阻抗值显著减小.在1 mol/L HAc-NaAc缓冲液中,利用循环伏安法和时间-电流曲线研究了SEM在CMWCNTs修饰电极上的电化学行为.SEM在修饰电极上呈现不可逆的氧化峰.与裸电极相比,氧化峰电流明显增大.在最佳实验条件(pH 7.0,扫描速度为0.1 V/s)下,测得SEM在5.00×10-6~1.09×10-3mol/L浓度范围内与氧化峰电流呈线性关系,线性方程为IP(μA)=-0.472+0.0599C(μmol/L),相关系数r=0.997,检出限为1.88×10-7 mol/L(S/N=3).在实际猪肝样品检测中加标回收率为92.8%~98.0%.

Rapid Detection of Semicarbazide Based on Glassy Carbon Electrode Modified with Carboxylated Multi-Walled Carbon Nanotubes

A sensitive electrochemical sensor for the detection of semicarbazide ( SEM ) based on the glassy carbon electrode modified with carboxylated multi-walled carbon nanotube ( CMWCNTs ) was constructed in this work. The modified materials were characterized by Fourier transform infrared spectroscopy, transmission electron microscopy and electrochemical impedance spectroscopy. The results showed that the CMWCNTs exhibited a certain degree of changes, such as the appearance of the characteristic peaks of carbon oxygen double bonds in carboxyl group, a decrease in diameter and length and a remarkable reduction of the impedance value. The electrochemical behavior of SEM on CMWCNTs/GCE was investigated by cyclic voltammetry and amperometric i-t curve in 1 mol/L HAc-NaAc buffer solution. An irreversible oxidation peak of SEM appeared at CMWCNTs/GCE. Compared to the bare electrode, the current of the oxidation peak was significantly increased. Under the optimal conditions such as HAc-NaAc solution ( pH 7 ) and scan rate of 0. 1 V/s, the obtained sensor presented linear response to SEM concentration in the range of 5. 0 × 10-6 mol/L-1. 09×10-3 mol/L, the linear regression equation was Ip(μA)=-0. 472+0. 0599C (μmol/L) with linear correlation coefficient of 0. 997. The detection limit was 1. 88×10-7 mol/L. At the same time, the recovery was from 92. 8% to 98. 0% in the test of pork liver samples.