韩 慧, 李锦州，孙仁霞

（哈尔滨师范大学 化学化工学院,黑龙江 哈尔滨 150025）

聚吡咯-酰基吡唑啉酮复合膜修饰玻碳电极测定酚磺乙胺的研究*

韩 慧, 李锦州**，孙仁霞

（哈尔滨师范大学 化学化工学院,黑龙江 哈尔滨 150025）

报道了一种新型聚吡咯-酰基吡唑啉酮复合膜修饰玻碳电极（Ppy/HPMαFP/GCE）对酚磺乙胺(ETH)电化学性质及其反应机理的研究。酚磺乙胺的电化学性质检测运用循环伏安法和脉冲伏安法。实验表明，与裸GCE和Ppy/GCE相比，Ppy/HPM αFP/GCE修饰电极对酚磺乙胺有良好的催化作用。聚吡咯与酰基吡唑啉酮产生了协同增效作用。在pH=5.5的磷酸盐(PBS)缓冲溶液中，该修饰电极测试ETH的CV曲线于0.35V和0.4V出现一对灵敏的氧化还原峰，峰电位差△Ep较裸玻碳电极降低510mV，比Ppy修饰电极降低100mV，峰电流显著增加。在最佳条件下, 氧化峰电流与ETH浓度于2.0×10-6～1.0×10-4mol·L-1范围内呈现良好的线性关系，检出限为6.0×10-7mol·L-1。

聚吡咯；酰基吡唑啉酮；酚磺乙胺；修饰电极

Abstract:In this paper,a novel voltammetric method using poly-pyrrole and acyl-pyrazolone composite film modified glassy carbon electrode(Ppy/HPMαFP/GCE)was developed for studying the electrochemical behavior and reaction mechanism of ethamsylate.The electrochemical parameters of ethamsylate were investigated by cyclic voltammetry and differential pulse voltammetry.Compared to the bare GCE and Ppy/GCE,the Ppy/HPMαFP/GCE showed an excellent electro-catalytical effect on the oxidation of ethamsylate with significant increase in the peak current.The above results indicated that a synergistic effect was existed between poly-pyrrole and HPMαFP.According to the experiment,In PBS buffer solution with a pH of 5.5,a pair of sensitive redox peaks with Epa=0.40V,Epc=0.35V(vs.SCE)was obtained on the PPy／HPMαFP modified electrode.The difference of peak potentials(△Ep)was 510mV which was lower than on bare glassy carbon electrode,and about 100mV lower than on Ppy modified electrode.Meanwhile,the peak current markedly increased.Under the optimum conditions,linear calibration curve was obtained in the concentration range of 2.0×10-6～1.0×10-4mol·L-1.The detection limit was 6.0×10-7mol·L-1.Key words:Poly-pyrrole;acyl-pyrazolone;ethamsylate;modified electrode

前 言

1 实验部分

1.1 仪器与试剂

电化学测试实验均在CHI 650A电化学工作站(上海辰华仪器公司，上海)上完成。采用三电极系统：饱和甘汞电极(SCE)为参比电极、铂电极为对电极、酰基吡唑啉酮 /聚吡咯修饰电极（HPMαFP/Ppy/GCE）(d=4mm)为工作电极。所有电位均相对于饱和甘汞电极。

吡咯(pyrrole简写py，国药集团化学试剂有限公司)；HPMαFP按文献[12]方法合成，以无水乙醇为溶剂配成浓度为1.0×10-2mol·L-1的溶液，备用；酚磺乙胺 (天津市大茂化学试剂厂)溶于水配制成1.0×10-3mol·L-1的标准溶液，用时稀释至所需浓度；磷酸盐缓冲溶液为 0.1 mol·L-1NaH2PO4和Na2HPO4两种溶液混合而成。其它试剂均为分析纯，实验用水为二次蒸馏水。……