基于Pd/g-C3N4-SWCNTs的雌二醇电化学传感器构建及应用研究  

Construction of a Palladium Nanoparticles/Graphitic Carbon Nitride Nanosheets-Single-walled Carbon Nanotubes Sensor and Its Application in Estradiol Detection

作　　者：郑志祥 王玫[2] 李江 宫雪[1] 王春明[3] ZHENG Zhi-xiang;WANG Mei;LI Jiang;GONG Xue;WANG Chun-ming(Gansu Province Key Laboratory of Evidence Science Techniques Research and Application,Gansu Institute of Political Science and Law,Lanzhou 730070,China;College of Pharmacy,Ningxia Medical University,Yinchuan 750004,China;College of Chemistry and Chemical Engineering,Lanzhou University,Lanzhou 730000,China)

机构地区：[1]甘肃省证据科学技术研究与应用重点实验室,甘肃政法学院,甘肃兰州730070 [2]宁夏医科大学药学院,宁夏银川750004 [3]兰州大学化学与化工学院,甘肃兰州730000

出　　处：《分析测试学报》2019年第10期1220-1227,共8页Journal of Instrumental Analysis

基　　金：国家自然科学基金项目(51862029);2019年陇原青年创新创业人才(团队)项目;甘肃政法学院重大科研项目(GZF2018XZD03);甘肃省引导科技创新发展专项资金项目(2018ZX-03)

摘　　要：利用表面具有丰富π电子的三聚氰胺(MAM)和单壁碳纳米管(SWCNTs)作为前驱体,通过固体研磨-热聚合法使二者通过π-π静电作用堆叠得到类石墨相氮化碳(Graphitic carbon nitride,g-C 3N 4)-SWCNTs复合材料,然后利用Na 2PdCl 4为Pd纳米粒子前体,通过自组装对g-C 3N 4-SWCNTs进行功能化修饰,得到Pd/g-C 3N 4-SWCNTs复合物。采用SEM、TEM、XRD、FTIR对该复合材料的形貌和组成进行表征,并利用循环伏安等电化学方法研究了该材料对雌二醇(E2)的电催化氧化性能。结果显示,雌二醇在Pd/g-C 3N 4-SWCNTs修饰电极上的响应电流明显大于其在g-C 3N 4、g-C 3N 4-SWCNTs修饰电极和裸玻碳电极上的响应。在优化实验条件下,采用示差脉冲伏安法考察了基质样品中E2的氧化峰电流与其浓度的关系,其氧化峰电流强度与其浓度在5~150μmol/L范围内呈良好的线性关系,线性方程为:I pa(μA)=0.834 7+0.007 0 C E2(r=0.990),检出限(LOD,S/N=3)为1.7μmol/L。该传感器具有良好的稳定性和选择性,且与HPLC在方法学上无显著性差异,可满足饲料样品中E2的检测需求。A palladium/graphitic carbon nitride(g-C3N4)-single-walled carbon nanotubes(SWCNTs)composite sensor was constructed for the detection of estradiol(E2).Firstly,the g-C3N4-SWCNTs were synthesized via solid grinding and followed by thermal polymerization with melamine(MAM)and single-walled carbon nanotube(SWCNTs)as precursors,then Pd nanoparticles were loaded on the as-prepared nanocomposite by self-assembly method.The morphology and composition of the Pd/g-C3N4-SWCNTs material were characterized by SEM,TEM,XRD and FTIR techniques,and its electrocatalytic performance toward estradiol(E2)was investigated by cyclic voltammetry.The Pd/g-C3N4-CNTs nanocomposite sensor was used for the detection of E2 in feedstuff sample.Under the optimum conditions,the DPV current response for E2 increased linearly in the concentration range of 5-150μmol/L with a linear equation of Ipa(μA)=0.834 7+0.007 0CE2(r=0.990)and a detection limit(LOD,S/N=3)of 1.7μmol/L.With good stability and selectivity,and no significant difference with the HPLC method,this method could meet the requirements for detection of E2 in feed samples.

关 键 词：类石墨相氮化碳 碳纳米管 雌二醇 电催化氧化 电化学分析 

分 类 号：O657.1[理学—分析化学] O629.8[理学—化学]