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作 者:陈纪文[1] 段成茜[1,2] 高作宁[1] 陈德刚
机构地区:[1]宁夏大学能源化工重点实验室,化学化工学院,银川750021 [2]宁夏医科大学高等卫生职业技术学院,银川750004 [3]宁夏多维泰瑞制药有限公司,银川750004
出 处:《分析化学》2012年第3期447-451,共5页Chinese Journal of Analytical Chemistry
基 金:宁夏自然科学基金(No.NZ1147)资助项目
摘 要:用乙炔黑(Acetylene black,AB)和离子液体(Ionic liquid,IL)制备了乙炔黑-离子液体复合修饰玻碳电极(AB-ILs/GCE),并用电化学阻抗谱(EIS)进行了表征。采用循环伏安法(Cyclic voltammetry,CV)和计时电流法(Chronoamperometry,CA),方波伏安法(Square wave voltammetry,SWV)研究了延胡索酸泰妙菌素(TF)在此电极上电化学行为及电化学动力学性质。结果表明,TF在玻碳电极(GCE)上于0.74 V处出现一个不可逆氧化峰,与GCE相比TF在AB/GCE上的氧化峰电位基本不变,氧化峰电流增大1.8倍;而与AB/GCE相比,TF在AB-ILs/GCE上的氧化峰电位略有负移,氧化峰电流增大3倍。实验结果表明,AB-ILs/GCE对TF电化学氧化有明显的催化作用。同时考察了实验条件对TF电化学行为的影响,测定了电极反应过程动力学参数,并用本方法对TF针剂中TF含量进行了定量测定,RSD在1.1%~2.9%之间,加标回收率在98.6%~101.8%之间。据此建立了TF电化学定量测定方法。Acetylene black-ionic liquid modified glassy carbon electrode(AB-ILs/GCE) was prepared by acetylene black Ionic liquid and characterized by electrochemical impedance spectroscopy(EIS).The electrochemical behaviors and electrochemical kinetics of tiamulin fumarate(TF) at AB-ILs/GCE were investigated by cyclic voltammetry(CV),chronoamperometry(CA) and Square Wave voltammetry(SWV).The experimental result showed an irreversible oxidation peak appeared on GCE at about 0.74V.However,the oxidation peak potentials of TF keep constant on AB/GCE than that of GCE,the oxidation peak currents on AB/GCE increased about 1.8 times than that of GCE;compared with AB/GCE,the oxidation peak potentials of TF on AB-ILs/GCE shifted 20mV negatively,the peak currents on AB-ILs/GCE increased 1.6 times than that of AB/GCE.The experimental result indicated that AB-ILs/GCE could catalyze the oxidation of TF well The electrochemical kinetic parameters were also determined on AB-ILs/GCE.The influence of experimental conditions was investigated.The quantitative determination of TF content was investigated,the relative standard deviation is between 1.1%-2.9% and the recoverage is in the range of 98.6%-101.8%.The method has been applied to the quantitative determination of TF content in injection sample.
关 键 词:电催化氧化 电分析方法 乙炔黑-离子液体修饰玻碳电极 延胡索酸泰妙菌素
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