RESUMO
In this work, we are pleased to present for the first time a 3D-printed electrochemical device using a lab-made conductive filament based on graphite (Gr) and polylactic acid (PLA) polymer matrix for the simultaneous detection of amoxicillin (AMX) and paracetamol (PAR). The sensor was properly characterized by scanning electron microscopy (SEM), electrochemical impedance spectroscopy (EIS), and cyclic voltammetry (CV). Compared to the commercial glassy carbon electrode (GCE), the superior performance of the 3D-Gr/PLA electrode was verified with a 3.8-fold more favored charge transfer. A differential pulse voltammetry (DPV) method was proposed providing a linear working range of 4 to 12 µmol L-1 for both analytes and a limit of detection (LOD) of 0.80 and 0.51 µmol L-1 for AMX and PAR, respectively. Additionally, repeatability studies (n = 5, RSD < 5.7%) indicated excellent precision, and recovery percentages ranging from 89 to 109% when applied to synthetic human urine, saliva, and plasma samples, attested to the accuracy of the method. The studies also indicate that the sensor does not suffer significant interference from common substances (antibiotics and biomarkers) present in the biological fluids, which makes it a promising analytical tool considering its low-cost, ease of manufacturing, robustness, and electrochemical performance.
Assuntos
Acetaminofen , Grafite , Humanos , Acetaminofen/química , Amoxicilina , Grafite/química , Eletrodos , Poliésteres , Impressão Tridimensional , Técnicas EletroquímicasRESUMO
In this work, the development of a disposable electrochemical device (US$ 0.02 per electrode) using a 3D printed support (3Ds) of acrylonitrile butadiene styrene (ABS) insulating filament with a composite material (CM) based on graphite and nail polish, immobilized on the support surface, was described for the electrochemical determination of diclofenac (DCF). The device was compared to the commercial glassy carbon electrode (GCE) and showed superior electroanalytical performance with approximately 1.8-fold higher current density. Additionally, an amperometric method for DCF determination in tap water, synthetic urine, and pharmaceutical formulation samples with the proposed electrode, using a flow injection analysis (FIA-AD) system, was developed. The optimized method presented excellent detectability (LOD = 0.47 µmol L-1), with excellent precision and accuracy (relative standard deviation < 5.6%) and percent recovery from spiked samples ranging from 89 to 106%. In addition, the sensor showed optimal analytical frequency with approximately 108 injections per hour, which demonstrates the potential of this system using the proposed disposable electrode for implementation in routine analysis and quality control with good selectivity and sensitivity.
Assuntos
Diclofenaco , Grafite , Diclofenaco/análise , Carbono , Água , Eletrodos , Técnicas Eletroquímicas/métodosRESUMO
A novel conductive filament based on graphite (Gr) dispersed in polylactic acid polymer matrix (PLA) is described to produce 3D-electrochemical devices (Gr/PLA). This conductive filament was used to additively manufacture electrochemical sensors using the 3D pen. Thermogravimetric analysis confirmed that Gr was successfully incorporated into PLA, achieving a composite material (40:60% w/w, Gr and PLA, respectively), while Raman and scanning electron microscopy revealed the presence of defects and a high porosity on the electrode surface, which contributes to improved electrochemical performance. The 3D-printed Gr/PLA electrode provided a more favorable charge transfer (335 Ω) than the conventional glassy carbon (1277 Ω) and 3D-printed Proto-pasta® (3750 Ω) electrodes. As a proof of concept, the ciprofloxacin antibiotic, a species of multiple interest, was selected as a model molecule. Thus, a square wave voltammetry (SWV) method was proposed in the potential range + 0.9 to + 1.3 V (vs Ag|AgCl|KCl(sat)), which provided a wide linear working range (2 to 32 µmol L-1), 1.79 µmol L-1 limit of detection (LOD), suitable precision (RSD < 7.9%), and recovery values from 94 to 109% when applied to pharmaceutical and milk samples. Additionally, the sensor is free from the interference of other antibiotics routinely employed in veterinary practices. This device is disposable, cost-effective, feasibly produced in financially limited laboratories, and consequently promising for evaluation of other antibiotic species in routine applications.
Assuntos
Ciprofloxacina , Grafite , Laboratórios , Análise Custo-Benefício , Técnicas Eletroquímicas/métodos , Grafite/química , Antibacterianos , Poliésteres/química , Impressão TridimensionalRESUMO
The emergence of bacteria genetically resistant to first- and second-generation fluoroquinolones has resulted in increased consumption of levofloxacin (LEV) in human and veterinary medicine. In this regard, the development of low cost and good sensitivity electrochemical devices has been highly required. Thus, in this work, we propose the development of a disposable electrochemical device (DED) using a lab-made conductive ink based on graphite powder and nail polish immobilized on a rigid polyvinyl chloride support (transparent sheet). Additionally, a simple and quick protocol for the electrodeposition of silver nanoparticles was used in order to improve the electroanalytical performance of the sensor (2.75-fold). A differential pulse voltammetry (DPV) method was optimized and the sensor was applied for LEV monitoring in pharmaceutical formulation samples, synthetic urine and simulated body fluid. The method showed a wide linear working range ranging from 0.5 to 50 µmol L-1 and a detection limit of 68.3 nmol L-1. Furthermore, the precision was adequate (RSD < 4.7%), while the accuracy was evaluated through spiked samples with percent recovery ranging from 93 to 103%. The sensor was also shown to be selective for LEV against other electroactive antibiotic species, thus demonstrating suitable characteristics for electroanalytical applications.