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  

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

作　　者：何保山[1] 杜耕安 

机构地区：[1]河南工业大学粮油食品学院,郑州450001

出　　处：《分析化学》2017年第10期1511-1516,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然基金项目(No.61301037);河南省科技开放合作项目(No.172106000014);河南省省属高校基本科研业务费专项资金项目(No.2014YWQQ05);河南工业大学青年骨干教师培育计划项目资助~~

摘　　要：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^(-3)mol/L浓度范围内与氧化峰电流呈线性关系,线性方程为I_P(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%。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（p H 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 I_P（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.

关 键 词：羧基化 多壁碳纳米管 玻碳电极 氨基脲 伏安法 

分 类 号：O657.1[理学—分析化学] TS251.9[理学—化学]