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• W2554486512 abstract "Molecularly imprinted polymers (MIPs) are artificial biomimetic receptors with applications in separation ranging from small molecules to whole cells. The combination of the MIP principle with conducting polymers allows the fabrication of specific and selective layers for sensing purposes. Not only the robustness of MIPs against environmental conditions and their low cost compared with natural receptors are advantages of MIPs, but also the possibility to prepare them for compounds which have no natural receptors. In this work, piezoelectric quartz crystals and analogous gold substrates were electrochemically coated with molecularly imprinted conducting polypyrrole films for pulsed amperometric detection (PAD) of clofibric acid, a metabolite of the blood lipid regulator clofibrate. Usually clofibric acid is detected by using reversed-phase HPLC with spectrophotometric detection. This requires large instrumentation, ultrapure solvents, and suitable sample preparation. An electrochemical sensing method would be advantageous due to the simple setup and low cost, and the use of organic solvents for the detection could be avoided. The films were prepared by cyclic voltammetry of an aqueous solution containing pyrrole as monomer, clofibric acid or, for feasibility studies, caffeine as template, and potassium chloride, potassium nitrate, or phosphate buffer solution as conducting salt. Non-imprinted polymers (NIPs) were prepared without template under the same conditions. The electrodeposition was monitored by a quartz crystal microbalance combined with an electrochemical cell. The deposition was influenced by the number of cycles and the applied potential, by the monomer concentration and the type of conducting salt, and also by the presence of the template. Cyclic voltammetry data obtained during polymerization and deposited weight estimations revealed a decrease of the polymerization rate with increasing clofibric acid concentration. Template entrapment and template removal were studied with X-ray photoelectron spectroscopy. The results indicated that clofibric acid could be removed after imprinting with an aqueous ethanol solution. Binding of caffeine and clofibric acid was studied with PAD. The results showed that optimizations of the washing procedure were needed. Washing procedures under stirring with frequent solvent change were tested with methanol, ethanol, and variation of the washing time, and were compared with washing by PAD measurements. In binding experiments, the highest sensor response to clofibric acid was obtained with sensors treated by PAD washing although the sensor response decreased gradually with repeated washing/measurement cycles. MIP and NIP surfaces were studied with atomic force microscopy (AFM), ellipsometry, contact angle measurements, and zeta potential measurements. AFM measurements revealed smooth surfaces with roughnesses of 6–8 nm for imprinted and non-imprinted layers. Differences between MIP and NIP layers were revealed by contact angle and zeta potential measurements. The results showed that contact angles were higher for MIPs than for NIPs and that the isoelectric point was lower for MIPs than for NIPs. Binding experiments with clofibric acid and other substances showed a pronounced selectivity of the MIP for clofibric acid vs. carbamazepine, but the response of MIP and NIP to the structurally related molecule 2,4-dichlorophenoxyacetic acid was higher than the response to clofibric acid. The smooth surface might be a reason for an excessively low density of specific binding sites for clofibric acid.Additionally to cyclic voltammetry, the application of potential pulses during polymerization was tested. Compared with cyclic voltammetry, the use of potential pulses resulted in more adherent films, which allowed testing the application of a negative potential as washing method.To introduce functional groups into the polymer, which could build more non-covalent bonds with the template during polymerization, pyrrole propionic acid and 2-(1H-pyrrole-1-yl)ethanamine were tested as monomers. Successful polymerization was obtained by copolymerization with pyrrole. The feasibility of sensor fabrication with a combination of molecular imprinting and electrochemical deposition of polypyrrole for the detection of clofibric acid could be demonstrated, but the specificity (response for MIP vs. NIP) and selectivity were strongly dependent on preparation and washing conditions." @default.
• W2554486512 created "2016-11-30" @default.
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• W2554486512 date "2016-03-03" @default.
• W2554486512 modified "2023-09-23" @default.
• W2554486512 title "Molecular imprinting of polypyrrole for electrochemical sensing of clofibric acid" @default.
• W2554486512 hasPublicationYear "2016" @default.
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