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This work focuses on the fabrication of non-enzymatic glucose sensing materials based on laser-formed Au nanoparticles embedded in Ti-textured substrates. Those materials possess good catalytic activity toward glucose oxidation in 0.1 × phosphate buffered saline as well as resistance to some interferants, such as ascorbic acid, urea, and glycine. The electrodes are further coated with three different polymers, that is, Nafion, photo-crosslinked poly(zwitterions) based on sulfobetaine methacrylate, and a hybrid membrane consisting of both polymers. Both the optimal integrity of the material and its catalytic activity toward glucose oxidation were maintained by the hybrid membranes with a large excess of poly(zwitterions) (mass ratio 20:1). The chemical structures of the as-formed membranes are confirmed by Fourier transform infrared spectroscopy. Due to the zwitterionic nature of the coating, the electrodes are resistant to biofouling and maintain electrochemical activity toward glucose for 4 days. Moreover, due to the synergistic effect of both Nafion and poly(zwitterions), the interference from the two compounds, namely, from acetylsalicylic acid and acetaminophen, was diminished. Besides the presence of polymer membranes, the electrode possesses a sensitivity of 36.8 μA cm-2 mM-1 in the linear range of 0.4-12 mM, while the limit of detection was estimated to be 23 μM. Finally, the electrodes are stable, and their response is not altered even by 1,000 bending cycles.

The detection of glucose at low concentrations using electrochemical sensors is of great importance due to the possibility of using different human body fluids than blood, such as e.g. urine, saliva, sweat or tears. The interest behind those biofluids is related to their utility in non-invasive sugar determination. In this work, we present flexible, fully biocompatible electrode material based on Au nanoparticles immobilized onto titanium dimples. Au Ti heterostructures were obtained via electrochemical anodization of titanium foil in presence of fluoride anions followed by chemical etching, magnetron sputtering of gold and subsequent thermal dewetting in continuous regime. In the last step of fabrication, electrodes were modified by permselective Nafion membrane. The selection of the best electrode material among different configurations was carried out basing on the electrochemical activity in the contact with 5 mM glucose dissolved in neutral air-saturated 0.1 M PBS. For the 10 nm Au dewetted gold film, limit of detection of 30 μM and high sensitivity of 93 mAcm 2mM 1 were achieved. Application of Nafion membrane caused complete inhibition of the impact of various interference species onto the glucose detection. Good selectivity and repeatability combined with the resistance to prolonged mechanical stress suggest that prepared material can be used in noninvasive glucose sensig

This paper focuses on the examination of glucose oxidation processes at an electrode material composed of gold nanoparticles embedded in a titanium template. Three different conditions were investigated: the chloride content in the electrolyte, its ionic conductivity and the presence of a Nafion coating. The impact of the provided environment on the oxidation reaction was evaluated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Two models, namely: chemisorption and incipient hydrous oxide/adatom mediator (IHOAM), were applied to explain the complex voltammetric responses of the electrodes exposed to solutions of varied glucose concentrations. Three different phenomena were observed for the studied cases. The first is related to the transition between the dominant mechanism of glucose oxidation from the IHOAM model to the chemisorption model. This happens only in an electrolyte containing chlorides after exceeding a certain amount of glucose. The second effect exhibits a bottleneck nature resulting from the presence of Nafion on the electrode&rsquo, s surface. In this case, mass transport through the semi-permeable polymer is hampered, due to the blocking of channels and physical internal cross-linking. This leads to a preconcentration of glucose inside the pores resulting in an increase in both the material sensitivity and the linear range of the calibration curve. Lastly, the third effect is manifested in a low concentration of the supporting electrolyte. It is based on the fact that mass transport of hydroxyl ions is governed not only by diffusion, but also by migration. These three effects have a tremendous impact on the glucose oxidation mechanism and reveal its very complex nature.

The synthesis of a potential immunosuppressant, i.e. dimethyl ester of N-mycophenoyl malonic acid was optimized in the reaction of mycophenolic acid (MPA) with amino malonic dimethyl ester in the presence of propanephosphonic anhydride (T3P) as a coupling reagent. The structural properties of the obtained MPA derivative were investigated by NMR, MS and single crystal X-ray diffraction methods. Theoretical considerations of conformational flexibility based on DFT calculations are presented.

We focus here on a novel approach to analysing the mechanisms of interference phenomena in glucose sensing, taking into account the changes within the Nafion layer deposited on the active surface. Several electrochemical techniques were used to verify the sustainability of catalytic properties of the electrode material after exposure to different compounds, i.e. ascorbic acid (AA), glycine, urea, acetylsalicylic acid (AsA), and acetaminophen (AAp). Through analysis of impedance data, we concluded that AAp and AsA were trapped permanently in the Nafion membrane, which significantly affected results repeatability. These observations were also confirmed by FT-IR investigations of the membrane after its immersion in solutions containing different interfering species. Moreover, after exposure to AsA and, unexpectedly, large concentrations of urea, the catalytic properties were completely lost, which, in consequence, make sensor reuse impossible. Such behaviour was justified by the chain reorganisation and swelling. Mechanisms involving adsorption onto the interphase and absorption in the membrane were proposed as key factors responsible for deterioration of membrane functionality and were confronted with FT-IR investigations. Following that, application of Nafion for non-invasive glucose sensor protection is unsatisfactory and cannot be considered for multiple detection procedures, especially taking into account biological fluids full of different interfering species.

This paper focuses on the synthesis route and electrochemical properties of electrocatalytic material based on gold nanoparticles (NPs) embedded in a structured titanium template obtained via optimized anodization, chemical etching and laser processing. SEM inspection reveals the presence of Au NPs (60–90 nm in diameter) sited in the titanium foil cavities. Performed electrochemical measurements enable nomination of the set of working laser parameters that allow for fabrication of material possessing the highest performance towards glucose oxidation. It is proven that laser-engineered electrodes have an improved stability in acidic conditions and higher response from glucose oxidation in both alkaline and neutral environment in comparison to analogs obtained by conventional furnace dewetting. In neutral electrolyte it is also observed that the current density increases by almost 300% while the change in mechanism of glucose oxidation was identified due to laser treatment. It is suggested that laser dewetted gold nanoparticles have more surface defects than furnace dewetted ones so that more AuOHads species are created and therefore catalytic activity of the material is enhanced. These results indicate a scalable and cost-effective fabrication route and are important for the current research on non-enzymatic glucose sensors.

This work focuses on the application of thermal analysis and kinetics investigations to analyze chemical processes during cross-linking of the complex fast-curing polyurethane system. Non-isothermal Differential Scanning Calorimetry (DSC) measurements were performed for both stoichiometric mixtures of polyol and isocyanate component and for mixture with large isocyanate excess. Isoconversional methods were used to calculate initial parameters for the multi-step procedure. Data were fitted according to autocatalytic Sestak-Berggren equation and activation energies and reaction orders were obtained. Those investigations led to the successful identification of three main reactions i.e. polyaddition, isocyanate deblocking and formation allophanate groups.