硬模板法制备氮掺杂有序介孔碳修饰电极检测盐酸奈福泮  

Preparation of N-doped Ordered Mesoporous Carbon Modified Electrode by Hard Template Method for Detection of Nefopam Hydrochloride

作　　者：程昊[1,3] 樊静静 刘永逸 CHENG Hao;FAN Jing-jing;LIU Yong-yi(Guangxi Liuzhou Luosifen Research Center of Engineering Technology,Guangxi Key Laboratory of Green Processing of Sugar Resources,College of Biological and Chemical Engineering,Guangxi University of Science and Technology,Liuzhou 545006,China;Liuzhou Institutes for Food and Drug Control,Liuzhou 545006,China;Province and Ministry Co-sponsored Collaborative Innovation Center of Sugarcane and Sugar Industry,Nanning 530004,China)

机构地区：[1]广西柳州螺蛳粉工程技术研究中心广西糖资源绿色加工重点实验室广西科技大学生物与化学工程学院,广西柳州545006 [2]柳州市食品药品检验所,广西柳州545006 [3]蔗糖产业省部共建协同创新中心,广西南宁530004

出　　处：《分析测试学报》2021年第7期1049-1054,共6页Journal of Instrumental Analysis

基　　金：中央引导地方科技发展专项“广西特色食品技术创新平台建设”项目;广西高等学校高水平创新团队及卓越学者计划资助项目(桂教人[2014] 7号);广西糖资源绿色加工重点实验室开放课题(GXTZY201701)

摘　　要：分别以三聚氰胺、尿素和乙二胺为氮源,阿拉伯糖为碳源,介孔硅(SBA-15)为模板剂,通过硬模板法成功制备了不同氮掺杂的介孔碳(N-CMK-3)。采用场发射扫描电镜(SEM)、透射电子显微镜(TEM)、全自动比表面及孔隙度分析仪(BET)、X射线衍射(XRD)、X射线光电子能谱(XPS)对不同材料进行表征。将N-CMK-3滴涂至玻碳电极表面构建电化学传感器,采用循环伏安法(CV)对N-CMK-3修饰电极的电化学行为进行考察。考察了修饰剂的用量和pH值对盐酸奈福泮电化学行为的影响。结果表明,在修饰剂量为6μL和pH 4.5的最佳实验条件下,盐酸奈福泮的氧化峰电流值与其浓度在1.0×10^(-8)~5.0×10^(-6)mol/L范围内呈良好的线性关系,r^(2)=0.992,检出限(S/N=3)为5.3×10^(-9)mol/L。此方法可用于盐酸奈福泮片的测定,加标回收率为95.9%~100%。Different N-doped mesoporous carbons(N-CMK-3)were prepared by hard template method,using melamine,urea and ethylenediamine as nitrogen source,arabinose as carbon source and mesoporous silicon(SBA-15)as template agent.The samples were characterized by scanning electron microscopy(SEM),transmission electron microscopy(TEM),brunner emmet teller(BET),X-ray diffraction(XRD)and X-ray photoelectron spectroscopy(XPS).The N-CMK-3 were coated onto glassy carbon electrodes to construct electrochemical sensors.The electrochemical characteristics of N-CMK-3 modified electrodes were investigated by cyclic voltammetry.Effects of amount of modifier and pH value on the electrochemical behavior of nefopam hydrochloride were investigated.The results showed that,under the optimal experimental conditions of 6μL modified dose and pH4.5,nefopam hydrochloride had a good linear relationship(r^(2)=0.992)between peak current and its concentration within 1.0×10^(-8)-5.0×10^(-6) mol/L.The limit of detection(LOD,S/N=3)was 5.3×10^(-9) mol/L.This method was applied to the detection of nafopam hydrochloride in human nafopam hydrochloride tablets,with recoveries of 95.9%-100%.

关 键 词：氮掺杂介孔碳 修饰电极 循环伏安法 盐酸奈福泮 

分 类 号：O657.7[理学—分析化学] TQ460.72[理学—化学]