基于石墨烯-壳聚糖修饰电极电化学测定4-壬基酚  

Electrochemical Determination of 4-Nonylphenol Based on Graphene-Chitosan Modified Glassy Carbon Electrode

作　　者：周文姝[1] 赵波[1] 黄晓华[1] 杨小弟[1] 

机构地区：[1]江苏省生物功能材料重点实验室江苏省新型动力电池重点实验室南京师范大学化学与材料科学学院,南京210097

出　　处：《分析化学》2013年第5期675-680,共6页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金资助项目(No.20875047);水利部专项基金资助项目(No.201201018);江苏高校优势学科建设工程资助项目

摘　　要：通过原位还原法制得GR-CS/GCE电极,对制得的电极用红外光谱、拉曼光谱进行表征,结果均表明氧化石墨烯被成功还原。采用循环伏安法和示差脉冲伏安法研究了4-NP的电化学行为,发现其氧化电流信号较GCE及GO-CS/GCE电极明显增强且电位负移,表明修饰电极对4-NP的氧化具有一定的催化作用。对富集电位、富集时间、扫速及缓冲溶液的pH等实验条件进行了优化,在最优条件下,4-NP的浓度与电流的线性响应范围为0.01～40.0μmol/L,线性回归方程为I(μA)=0.364C(μmol/L)+0.618(R=0.9988),检出限为5.2 nmol/L(S/N=3),将该电极用于实际样品中4-NP检测,加标回收率为95.0%～101.0%。A grapheme-chitosan modified glassy carbon electrode （GR-CS/GCE） was prepared by in situ reduction and characterized by Fourier transform-infrared （FF-IR） spectra and Raman spectra. The results showed that the graphene oxide （GO） was successfully deoxygenized. On the basis of this, the electrochemical behavior of 4-nonylphenol （4-NP） was investigated by cyclic voltammetry and differential pulse voltammetry. It was found that the oxidation current at GR-CS/GCE electrode was obviously larger＇ than that at GCE electrode and GO-CS/GCE electrode, and the oxidation potential shifted negatively, indicating that the GR- CS/GCE electrode had obviously catalytic activity on the 4-NP＇s oxidation. Experimental parameters, such as accumulation potential and time, scan rate, and pH value of buffer solution were optimized. Under the optimized conditions, the oxidation peak current was proportional to 4-NP concentration in the range between 0.01 and 40.0 μmol/L, the linear equation was I （μA） = 0. 364C（μmol/L） ＋ 0. 618 （R = 0. 9988 ） and the detection limit was 0. 0052 μmol/L （S/N= 3 ）. Finally, this proposed sensor was successfully employed to determine the 4-NP in real samples and the recoveries were between 95.0% and 101.0%.

关 键 词：石墨烯 4-壬基酚 电化学检测 示差脉冲伏安法 

分 类 号：O657.1[理学—分析化学]