Grupo de Pesquisa em Macromoléculas e Interfaces - Departamento de Química, Universidade Federal do Paraná, C.P. 19032, Curitiba, 81531-980, Brazil.
Grupo de Cromatografia e Técnicas de Microextração - Departamento de Química, Universidade Federal do Paraná, C.P. 19032, Curitiba, 81531-980, Brazil.
Mikrochim Acta. 2019 Jun 10;186(7):398. doi: 10.1007/s00604-019-3545-z.
Polypyrrole (PPy) was electrochemically synthesized with charge control on the surface of a steel mesh. Two different morphologies (globular and nanotubular) were created and characterized by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The modified electrodes were used as extraction phases in solid-phase extraction (SPE) and electrochemically controlled solid-phase extraction (EC-SPE) of atrazine, caffeine and progesterone. Raman spectroscopy was employed for the structural characterization of PPy after long exposure to the analytes. The electrochemical behavior was studied by cyclic voltammetry which revealed the higher capacitive behavior of polypyrrole nanotubes because of the huge superficial area, also no electrocatalytical behavior was observed evidencing the strong adsorption of the analytes on the PPy surface. The effects of the PPy oxidation state on the extraction performance were evaluated by in-situ electrochemical sorption experiments. The sorption capacity was evaluated by gas chromatography coupled to mass spectrometry (GC-MS). The method displays good stability, repeatability and reproducibility. The limits of detection range between 1.7-16.7 μg L. Following the extraction of river water samples, it was possible to identify the presence of other endogenous organic compounds besides the analytes of interest. This indicates the potential of the method and material developed in this work. Graphical abstract Schematic representation of a steel mesh electrode covered with polypyrrole nanotubes used as extraction phase for separation of contaminants from aqueous samples. The oxidation level of polypyrrole was electrochemically tuned by which the adsorption of analytes is deeply affected.
聚吡咯(PPy)通过在钢丝网上的表面电荷控制电化学合成。通过扫描电子显微镜(SEM)和透射电子显微镜(TEM)对两种不同的形态(球形和纳米管状)进行了创建和表征。改性电极被用作固相萃取(SPE)和电化学控制固相萃取(EC-SPE)中莠去津、咖啡因和孕酮的萃取相。拉曼光谱用于研究 PPy 在长时间暴露于分析物后的结构特征。电化学行为通过循环伏安法进行研究,结果表明聚吡咯纳米管具有更高的电容行为,因为其具有巨大的比表面积,同时也没有观察到电催化行为,这表明分析物在 PPy 表面的强烈吸附。通过原位电化学吸附实验评估了 PPy 氧化态对萃取性能的影响。通过气相色谱-质谱联用(GC-MS)评估了吸附容量。该方法显示出良好的稳定性、重复性和重现性。检测限范围在 1.7-16.7μg/L 之间。在对河水样品进行萃取后,除了感兴趣的分析物外,还可以识别出其他内源性有机化合物的存在。这表明了该方法和所开发材料的潜力。