RESUMO
Fentanyl is a powerful synthetic opioid used to treat severe pain. New administration routes toward its illegal consumption for recreational purposes pose a growing threat to public health, either due to misuse or abuse of this substance. As a result, the rapid qualitative and quantitative determination of fentanyl in biofluids is of great interest. A novel enzymatic biosensor based on adsorptive-stripping cyclic voltammetry is proposed as a cost-effective, reliable, and efficient device for fentanyl determination in urine samples. Disposable screen-printed carbon electrodes modified with multi-walled carbon nanotubes and cytochrome c were used to develop the testing platform. The electrochemical behavior of fentanyl exhibited a well-defined anodic wave around 0.66 V vs. pseudo reference electrode. The experimental conditions were optimized to obtain the best analytical response, and linear regression analysis of increasing concentration standards was applied to estimate the performance parameters. The results suggest a simple method with a wide linearity range, high sensitivity, low limits of detection (0.086 µg/mL) and quantification, and satisfactory precision (2.9% RSD). The feasibility and applicability of the voltammetric approach were assessed by fentanyl-spiked urine samples by standard additions calibration curves in two levels of enrichment with an accuracy of 92% and 100%.
Assuntos
Técnicas Biossensoriais , Nanotubos de Carbono , Citocromos c , Fentanila , EletrodosRESUMO
A novel amperometric biosensor for the determination of Al(III) based on the inhibition of the enzyme superoxide dismutase has been developed. The oxidation signal of epinephrine substrate was affected by the presence of Al(III) ions leading to a decrease in its amperometric current. The immobilization of the enzyme was performed with glutaraldehyde on screen-printed carbon electrodes modifiedwith tetrathiofulvalene (TTF) and different types ofnanoparticles. Nanoparticles of gold, platinum, rhodium and palladium were deposited on screen printed carbon electrodes by means of two electrochemical procedures. Nanoparticles were characterized trough scanning electronic microscopy, X-rays fluorescence, and atomic force microscopy. Palladium nanoparticles showed lower atomic force microscopy parameters and higher slope of aluminum calibration curves and were selected to perform sensor validation. The developed biosensor has a detection limit of 2.0 ± 0.2 µM for Al(III), with a reproducibility of 7.9% (n = 5). Recovery of standard reference material spiked to buffer solution was 103.8% with a relative standard deviation of 4.8% (n = 5). Recovery of tap water spiked with the standard reference material was 100.5 with a relative standard deviation of 3.4% (n = 3). The study of interfering ions has also been carried out.
RESUMO
A novel amperometric biosensor for the determination of Al(III) based on the inhibition of the enzyme acetylcholinesterase has been developed. The immobilization of the enzyme was performed on screen-printed carbon electrodes modified with gold nanoparticles. The oxidation signal of acetylthiocholine iodide enzyme substrate was affected by the presence of Al(III) ions leading to a decrease in the amperometric current. The developed system has a detection limit of 2.1 ± 0.1 µM for Al(III). The reproducibility of the method is 8.1% (n = 4). Main interferences include Mo(VI), W(VI) and Hg(II) ions. The developed method was successfully applied to the determination of Al(III) in spiked tap water . The analysis of a certified standard reference material was also carried out. Both results agree with the certified values considering the respective associated uncertainties.
Assuntos
Acetilcolinesterase/química , Alumínio/análise , Técnicas Biossensoriais/instrumentação , Condutometria/instrumentação , Ouro/química , Nanopartículas Metálicas/química , Água/química , Alumínio/química , Inibidores da Colinesterase/análise , Inibidores da Colinesterase/química , Desenho de Equipamento , Análise de Falha de Equipamento , Nanopartículas Metálicas/ultraestrutura , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , SoluçõesRESUMO
En este artículo se revisan las principales evidencias de la neurotoxicidad in vitro del aluminio, y algunos hallazgos en cerebros de pacientes de la enfermedad de Alzheimer, se muestran algunos estudios realizados con pacientes que sufren deficiencias renales, como los tipos más importantes de ostodistrofias causados por aluminio. El problema de analizar la baja concentración de aluminio presente en fluidos humanos se resuelve con métodos analíticos muy sensibles como la espectrofotometría electrotérmica de absorción atómica ETAS, y métodos voltamperométricos con agentes acomplejantes; que permiten adsorción sobre electrodos sólidos o de gota suspendida de mercurio. Es muy importante conocer con exactitud la concentración de aluminio en agua usada en para preparar las disoluciones usadas en la hemodiálisis, o en las disoluciones usadas en la diálisis peritoneal ambulatoria, como primer paso para evitar la contaminación de los pacientes con aluminio. La prevención de la contaminación durante el muestreo, almacenaje y análisis de fluidos dializados es prioritaria y el agua usada en diálisis debe ser tan baja como sea posible en contenido de por aluminio.
This article reviews the principal evidences about aluminum neurotoxicity in vitro, and some evidences in brain tissues of Alzheimer patients; and also show some studies realized with humans that suffer renal deficiencies, dealing with the principal osteodystrophy. The problem of analyzing low aluminum concentration in human fluids is overcomed with very sensitive analytical methods as Electrothermal Atomic Absorption Spectrometry (ETAS) and voltammetric methods as Anodic Striping Voltammetry with complexing agents that easing adsorption over solid electrodes or mercury hanging drop. Is a vital question to know with accuracy the aluminum concentration in water used in hemodialysis or in fluids used in ambulatory peritoneal dialysis, as a first stage to prevent contamination by aluminium. So the prevention of contamination during sampling, storage and analysis of biological fluids should be the first need and the sources of water used in renal dialysis keep be as clean as possible of aluminium contamination.