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基于Pd/g-C3N4-SWCNTs的雌二醇电化学传感器构建及应用研究
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郑志祥,王玫,李江,宫雪,王春明 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2.宁夏医科大学药学院3.兰州大学化学与化工学院 
基金项目: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)
中文摘要: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-C3N4)-SWCNTs复合材料,然后利用Na2PdCl4为Pd纳米粒子前体,通过自组装对g C3N4-SWCNTs进行功能化修饰,得到Pd/g C3N4-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-C3N4-SWCNTs修饰电极上的响应电流明显大于其在g C3N4、g-C3N4-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5~150 μmol/L范围内呈良好的线性关系,线性方程为:Ipa(μA)=0.834 7+0.007 0CE2(r=0.990),检出限(LOD,S/N=3)为1.7 μmol/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。
中文关键词:类石墨相氮化碳  碳纳米管  雌二醇  电催化氧化  电化学分析
 
Construction of a Palladium Nanoparticles/Graphitic Carbon Nitride Nanosheets-Single walled Carbon Nanotubes Sensor and Its Application in Estradiol Detection
Abstract: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 5-150 μmol/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 1.7 μmol/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.
Key Words:graphitic carbon nitride nanosheets  carbon nanotubes  estradiol  electrochemical
引用本文:郑志祥,王玫,李江,宫雪,王春明.基于Pd/g-C3N4-SWCNTs的雌二醇电化学传感器构建及应用研究[J].分析测试学报,2019,38(10):1220-1227.
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