We report for the first time a procedure in which Nafion/Graphite nanoplatelets (GNPs) thin films are fabricated using a modified layer-by-layer (LbL) method. The method consists of dipping a substrate (quartz and/or glassy carbon electrodes) into a composite solution made of Nafion and GNPs dissolved together in ethanol, followed by washing steps in water. This procedure allowed the fabrication of multilayer films of (Nafion/GNPs)_n by means of hydrogen bonding and hydrophobic‒hydrophobic interactions between Nafion, GNPs, and the corresponding solid substrate. The average thickness of each layer evaluated using profilometer corresponds to ca. 50 nm. The as-prepared Nafion/GNPs LbL films were characterized using various spectroscopic techniques such as X-ray photoelectron spectroscopy (XPS), energy-dispersive X-ray spectroscopy (EDS), FTIR, and optical microscopy. This characterization highlights the presence of oxygen functionalities that support a mechanism of self-assembly via hydrogen bonding interactions, along with hydrophobic interactions between the carbon groups of GNPs and the Teflon-like (carbon‒fluorine backbone) of Nafion. We showed that Nafion/GNPs LbL films can be deposited onto glassy carbon electrodes and utilized for the voltammetric detection of caffeine in beverages. The results showed that Nafion/GNPs LbL films can achieve a limit of detection for caffeine (LoD) of 0.032 μM and linear range between 20‒250 μM using differential pulse voltammetry, whereas, using cyclic voltammetry LoD and linear range were found to be 24 μM and 50‒5000 μM, respectively. Voltammetric detection of caffeine in beverages showed good agreement between the values found experimentally and those reported by the beverage producers. The values found are also in agreement with those obtained using a standard spectrophotometric method. The proposed method is appealing because it allows the fabrication of Nafion/GNPs thin films in a simple fashion using a single-step procedure, rather than using composite solutions with opposite electrostatic charge, and also allows the detection of caffeine in beverages without any pre-treatment or dilution of the real samples. The proposed method is characterized by a fast response time without apparent interference, and the results were competitive with those obtained with other materials reported in the literature.

We describe a fast and reliable procedure for the efficient extraction of nitrites in cured meat using microwave-assisted heat and report their in situ determination via voltammetry using an anion-exchanger ionene, hexamethyl-p-terphenyl poly(benzimidazolium) (HMT-PMBI), and nitrogen-doped graphite nanoplatelets (NGNPs). Cyclic voltammetry and chronoamperometry were utilized to evaluate the concentration of the redox mediator within the film and apparent diffusion coefficient. To investigate the suitability of the composite material for sensing applications, HMT-PMBI/NGNPs were tested for their detection of nitrite in bacon samples without the need of any pretreatments or dilutions. HMT-PMBI/NGNP coated electrodes showed enhanced sensitivity in the detection of nitrite ions in bacon with a limit of detection (LoD) of 0.64 µM, sensitivity 0.52 µA µM⁻¹ cm⁻², and operating in a linear range between 1–300 μM. The results highlight that the determination of nitrites in cured meat using microwave extraction is in good agreement with standard procedures such as the ISO 2918 and the AOAC International 973.31 methods.