RESUMO
Molybdenum disulfide (MoS2) surface functionalization was performed with a catechol-containing polymer sodium alginate (SA) and dopamine (DA) through simultaneous MoS2 exfoliation and self-polymerization of DA. The MoS2/SA-PDA nanocomposite was characterized using spectroscopic, microscopic, and electroanalytical techniques to evaluate its electrocatalytic performance. The electrocatalytic behavior of the MoS2/SA-PDA nanocomposite modified electrode for the detection of acebutolol (ACE), a cardio-selective ß-blocker drug was explored through cyclic voltammetric and differential pulse voltammetric techniques. The influence of scan rate, concentration, and pH value on the oxidation peak current of ACE was investigated to optimize the deducting condition. The electrochemical activity of the MoS2/SA-PDA nanocomposite electrode was attributed to the existence of reactive functional groups being contributed from SA, PDA, and MoS2 exhibiting a synergic effect. The MoS2/SA-PDA nanocomposite modified electrode exhibits admirable electrocatalytic activity with a wide linear response range (0.009 to 520 µM), low detection limit (5 nM), and high sensitivity (0.354 µA µM-1 cm-2) also in the presence of similar (potentially interfering) compounds. The fabricated MoS2/SA-PDA nanocomposite modified electrode can be useful for the detection of ACE in pharmaceutical analysis.
Assuntos
Acebutolol/análise , Antagonistas de Receptores Adrenérgicos beta 1/análise , Técnicas Biossensoriais/instrumentação , Técnicas Eletroquímicas/instrumentação , Nanocompostos/química , Acebutolol/sangue , Acebutolol/química , Acebutolol/urina , Antagonistas de Receptores Adrenérgicos beta 1/sangue , Antagonistas de Receptores Adrenérgicos beta 1/química , Antagonistas de Receptores Adrenérgicos beta 1/urina , Alginatos/química , Técnicas Biossensoriais/métodos , Dissulfetos/química , Técnicas Eletroquímicas/métodos , Eletrodos , Humanos , Indóis/química , Limite de Detecção , Molibdênio/química , Oxirredução , Polímeros/química , Reprodutibilidade dos TestesRESUMO
In this work, a graphene oxide (GRO)-based temperature-sensitive smart catalytic support material was developed by tethering biodegradable and hydrophilic poly(N-vinylcaprolactam) (PVCL) on a GRO (i.e., GRO-PVCL) surface. GRO-PVCL-supported palladium catalyst (i.e., Pd/GRO-PVCL) was then prepared for tizanidine (TZN) electroreduction. The impact of a temperature-sensitive smart surface on the electrochemical and electrocatalytic properties was examined. Moreover, when the large surface area, excellent electron transfer, and electrochemical catalysis abilities of GRO were combined with the responsive characteristics of PVCL, temperature-triggered reversible electrocatalysis of TZN with enhanced sensitivity has been proved. Results designated that GRO-PVCL exposed the hydrophilic surface at 20 °C, resulting in Pd NPs highly dispersed on the GRO-PVCL surface. Subsequently, the wettability of the Pd catalyst surface arbitrarily adapted to hydrophobicity at 40 °C, which highly enhanced the TZN reduction on the catalyst in electrochemical detection. The synergistic effect amid Pd and GRO-PVCL on Pd/GRO-PVCL improved the electrocatalytic activity of TZN. The detection of TZN with the Pd/GRO-PVCL modified electrode ranged from 0.02 to 276 µM with a low detection limit of 0.0015 µM at 40 °C. The Pd/GRO-PVCL modified electrode also possesses excellent stability, reproducibility, and anti-interference ability. Lastly, the modified electrode attained good recovery results in human urine and human plasma samples for the determination of TZN and also pharmacokinetics study in rat plasma.
Assuntos
Clonidina/análogos & derivados , Técnicas Eletroquímicas/métodos , Grafite/química , Paládio/química , Caprolactama/análogos & derivados , Caprolactama/química , Catálise , Clonidina/análise , Clonidina/química , Eletrodos , Interações Hidrofóbicas e Hidrofílicas , Limite de Detecção , Nanocompostos/química , Polímeros/química , Reprodutibilidade dos Testes , Propriedades de Superfície , TemperaturaRESUMO
A 3D flexible domestic waste styrofoam is reported as a surface enhanced Raman scattering (SERS) substrate loaded with BiOCl-BiOBr@Pt/Au semiconductor-plasmonic composites. The hydrothermally prepared BiOCl-BiOBr nanocomposite is thoroughly characterized for its crystal structure using X-Ray diffraction, morphology through scanning electron microscopy, and electronic states of the elements using X-ray photoelectron spectroscopy. The alpha cypermethrin (ACM) is chosen as a model pesticide analyte for SERS investigation. The BiOCl-BiOBr@Pt/Au loaded foam substrate exhibited a high enhancement factor (106) and low limit of detection (10-10 M) upon SERS investigation. The unique architecture of the semiconductor-plasmonic composite enables an efficient charge transfer capability and plasmonic hotspots which aids in the enhancement of target analytes. In order to better demonstrate the versatility towards other pesticides, SERS detection of glyphosate and paraquat pesticides are also performed using the fabricated SERS substrate. The stability of the substrate has been investigated in detail for 30 days and the substrate was highly stable. The BiOCl-BiOBr@Pt/Au-based foam substrate also performed well in rapid real-time sensing of alpha cypermethrin on the kiwi fruit exocarp at lower level concentrations. Graphical abstract.
Assuntos
Nanopartículas Metálicas/química , Praguicidas/química , Poliestirenos/química , Humanos , Prata/químicaRESUMO
Lanthanum oxide nanomaterials were decorated with carbon black (CB) and grafted with a poly(acrylic acid) nanogel to obtain a composite material (CB-g-PAA/La2O3) for simultaneous determination of acetaminophen (AMP), naproxen (NPX), and theophylline (TPH). The nanogel was synthesized by in-situ free radical polymerization. The composite was dropped onto a glassy carbon electrode (GCE), and the modified GCE displays robust electrocatalytic activity towards AMP, NPX, and TPH, with voltammetric signals that are enhanced compared to a bare GCE. Features of merit for AMP, NPX, and TPH, respectively, include (a) peak potentials of 0.42, 0.85 and 0.12 V (vs. Ag/AgCl), (b) linear ranges from 0.05-887, 0.05-884, and 0.02-888 µM, and (c) detection limits of 20, 35, and 15 nM. The practical applicability of the CB-g-PAA/La2O3/GCE was illustrated by analyzing serum and urine samples. Graphical abstract Schematic presentation of simultaneous electrochemical sensing of acetaminophen (AMP), naproxen (NPX), and theophylline (TPH) in real sample analysis using poly(acrylic acid) nanogel covalently grafted onto a carbon black/La2O3 composite (CB-g-PAA/La2O3/GCE).
Assuntos
Acetaminofen/análise , Resinas Acrílicas/química , Lantânio/química , Nanogéis/química , Naproxeno/análise , Óxidos/química , Fuligem/química , Teofilina/análise , Acetaminofen/sangue , Acetaminofen/urina , Eletroquímica , Eletrodos , Humanos , Modelos Moleculares , Conformação Molecular , Naproxeno/sangue , Naproxeno/urina , Polimerização , Teofilina/sangue , Teofilina/urinaRESUMO
A one-pot synthesis method for the fabrication of biomass-derived activated carbon-zinc oxide (ZAC) nanocomposites using sugarcane bagasse as a carbon precursor and ZnCl2 as an activating agent is reported. For the first time, we used ZnCl2 as not only an activating agent and also for the synthesis of ZnO nanoparticles on the AC surface. ZAC materials with varying ZnO loading were prepared and characterized by a variety of analytical and spectroscopic techniques such as FE-SEM, FE-TEM, XRD, EA, XPS, and Raman spectroscopy. ZAC-modified glassy carbon electrodes (GCEs) were found to exhibit remarkable electrochemical properties for simultaneous detection of ascorbic acid (AA), dopamine (DA), and uric acid (UA) as well as hazardous pollutants such as hydrogen peroxide (H2O2) and hydrazine (N2H4) with desirable sensitivity, selectivity, and detection limits. Moreover, ZAC-modified stainless steel electrodes also showed superior performances for supercapacitor applications. The ZAC nanocomposites, which may be mass produced by the reported facile direct route from sugarcane bagasse, are not only eco-friendly but also cost-effective, and thus, are suitable as a practical platform for bio-sensing and energy storage applications.
Assuntos
Técnicas Biossensoriais , Carbono/química , Fontes de Energia Elétrica , Nanocompostos/química , Óxido de Zinco/química , Ácido Ascórbico/análise , Celulose/química , Cloretos/química , Dopamina/análise , Capacitância Elétrica , Eletrodos , Química Verde , Hidrazinas/análise , Peróxido de Hidrogênio/análise , Limite de Detecção , Tamanho da Partícula , Porosidade , Saccharum , Ácido Úrico/análise , Compostos de Zinco/química , Óxido de Zinco/síntese químicaRESUMO
A simple method to immobilize poly(neutral red) (PNR) and flavin adenine dinucleotide (FAD) hybrid film (PNR/FAD) by cyclic voltammetry is proposed. The PNR/FAD hybrid film can be easily prepared on an electrode surface involving electropolymerization of neutral red (NR) monomers and the electrostatic interaction between the positively charged PNR and the negatively charged FAD. It exhibits electroactive, stable, surface-confined, pH-dependent, nano-sized, and compatible properties. It provides good electrocatalytic properties to various species. It shows a sensitivity of 5.4 µA mM(-1) cm(-2) and 21.5 µA mM(-1) cm(-2) for hydrogen peroxide (H(2)O(2)) and nicotinamide adenine dinucleotide (NADH) with the linear range of 0.1 µM-39 mM and 5 × 10(-5) to 2.5 × 10(-4) M, respectively. It shows another linear range of 48.8-355.5 mM with the sensitivity of 12.3 µA mM(-1) cm(-2) for H(2)O(2). In particular, the PNR/FAD hybrid film has potential to replace some hemoproteins to be a cathode of biofuel cells and provide the biosensing system for glucose and ethanol.
Assuntos
Técnicas Biossensoriais/métodos , Flavina-Adenina Dinucleotídeo/química , Peróxido de Hidrogênio/análise , NAD/análise , Vermelho Neutro/química , Polímeros/química , Álcoois/análise , Álcoois/química , Sítios de Ligação , Técnicas Biossensoriais/instrumentação , Catálise , Corantes/química , Corantes/metabolismo , Eletroquímica , Eletrodos , Flavina-Adenina Dinucleotídeo/metabolismo , Glucose/análise , Glucose/química , Peróxido de Hidrogênio/química , Concentração de Íons de Hidrogênio , NAD/química , Nanocompostos/química , Vermelho Neutro/metabolismo , Oxirredução , Polímeros/metabolismo , Sensibilidade e EspecificidadeRESUMO
Pharmaceutical wastes, acetaminophen (AP) widely used in medical fields, is often discharged into water, causing harm to human health. Hence, there is an urgent need to effectively remove AP from wastewater systems. In this paper, polypyrrole (PPy) composite with MoO3 has been synthesized via an in-situ polymerization method. The as-prepared materials were thoroughly characterized by XRD, FT-IR, UV-DRS, SEM, TEM and mapping techniques. The as-prepared MoO3@PPy composite was utilized to removal of AP via photocatalytic degradation and electrochemical determination. Under optimized composite, MoO3@PPy (2) showed an excellent photocatalytic degradation and electrochemical determination of AP compared to pure MoO3 and all other composites. The higher catalytic activity was ascribed to the effective interfacial charges transfer, reduce the recombination and enhance the active surface area of electrode via a synergistic effect. The photocatalytic degradation mechanism, rate and kinetic of the reaction were investigated and discussed. The major active degradation species and an effective charge transfer properties were confirmed by trapping experiments and photocurrent spectra. In addition, the MoO3@PPy (2) modified GCE exhibit the AP determination activity by DPV with a linear range of 0.05-546 µM. The limit of detection and sensitivity of electrode were 0.0007 µM and 0.242 µM-1 cm-2 respectively. Moreover, the proposed electrode showed good selectivity, stability and reproducibility. This method was useful for the determination of AP in real samples.
Assuntos
Polímeros , Pirróis , Acetaminofen , Eletrodos , Humanos , Reprodutibilidade dos Testes , Espectroscopia de Infravermelho com Transformada de FourierRESUMO
Electrically conductive polymer nanomaterials signify a promising class of sensing platforms in the field of electrochemistry, but their applications as electrocatalysts are commonly limited by their poor colloidal stability in aqueous media and large particle sizes. Inspired by biomineralization approaches for integrating nanoscale materials, herein, a gadolinium (Gd)-integrated polypyrrole (PPy) electrocatalyst (namely, BSA@PPy-Gd) was successfully prepared by choosing bovine serum albumin (BSA) as a stabilizer for biomimetic mineralization and polymerization in a "one-step" manner. BSA@PPy-Gd possesses outstanding water dispersibility, nanoscale morphology, and improved electrical conductivity. The electrocatalytic competency of the electrochemical (EC) sensing platform fabricated for the sensitive detection of nicardipine (NCD) was assessed. The synergy of remarkable conductivity, superior active surface area, and electrostatic interactions stimulated by the combination of BSA with the NH group of PPy on BSA@PPy-Gd and Gd increases the fast electron transfer at the analyte-electrode junction. The fabricated EC sensor, BSA@PPy-Gd/glassy carbon electrode (GCE), exhibits a current intensity greater than that of PPy/GCE, BSA/GCE, and bare GCE in terms of peak height at a pH of 7.0 in phosphate buffer solution. The newly fabricated EC sensing platform shows excellent electrocatalytic activities for the electroreduction of NCD in terms of a low detection limit (2 nM), good sensitivity, linear dynamic detection ranges (0.01-575 µM), operational stability, and repeatability and was also tested on rat and human serum specimens.
Assuntos
Polímeros , Pirróis , Animais , Biomimética , Eletrodos , Gadolínio , Nicardipino , RatosRESUMO
Electrochemically active composite film that contains multiwalled carbon nanotubes (MWCNTs), Nafion (NF), and poly(malachite green) (PMG) has been synthesized on glassy carbon electrode (GCE), gold, and indium tin oxide (ITO) electrodes by potentiodynamic method. The presence of MWCNTs in the composite film (MWCNT-NF-PMG) enhances the surface coverage concentration (Γ) of PMG by fivefold. Similarly, an electrochemical quartz crystal microbalance study revealed enhancement in the deposition of PMG at MWCNT-NF film when compared with bare and only NF modified electrodes. The surface morphology of the composite film was studied using atomic force microscopy, which revealed that the PMG incorporated on MWCNT-NF film. The composite film exhibited enhanced electrocatalytic activity toward the mixture of biochemical compounds catechol and quinol. The electrocatalytic responses of analytes at MWCNT-NF-PMG composite film were measured using both cyclic voltammetry (CV) and differential pulse voltammetry (DPV). From electrocatalysis studies, well-separated voltammetric peaks were obtained at the composite film for catechol and quinol with a peak separation of 147mV. The sensitivity values of the composite film toward catechol and quinol by the DPV technique were 0.4 and 3.2mAmM(-1)cm(-2), respectively, which are higher than the values obtained by the CV technique. Similarly, the above-mentioned values are better than the previously reported electroanalytical values for the same analytes.
Assuntos
Catecóis/análise , Técnicas Eletroquímicas/métodos , Hidroquinonas/análise , Nanotubos de Carbono/química , Polímeros/química , Corantes de Rosanilina/química , Carbono/química , Catálise , Eletrodos , Polímeros de Fluorcarboneto/química , Vidro/química , Concentração de Íons de Hidrogênio , Limite de Detecção , Microscopia de Força Atômica , Nanotubos de Carbono/ultraestrutura , Oxirredução , PolimerizaçãoRESUMO
Herein, a hierarchical structure of flower-like NiCo layered double hydroxides (NiCo LDH) microspheres composed of three-dimensional (3D) ultrathin nanosheets was successfully synthesized via a facile hydrothermal approach. The formation of NiCo LDH was confirmed by various physicochemical studies, and the NiCo LDH-modified glassy carbon electrode was used as an efficient dual-functional electrocatalyst for non-enzymatic glucose and hydrogen peroxide (H2O2) biosensor. The host matrix of hydrotalcite NiCo LDH exhibits the enhanced electrocatalytic sensing performances with a quick response time (<3 s), wide linear range (50 nM-18.95 mM and 20 nM-11.5 mM) and lowest detection limits (S/N = 3) (10.6 and 4.4 nM) toward glucose and H2O2, and also it exhibits good stability, selectivity, and reproducibility. In addition, this biosensor was successfully utilized to the real-time detection of endogenous H2O2 produced from live cells and glucose in various biological fluids, and demonstrates that the as synthesized NiCo LDH may provide a successful pathway for physiological and clinical pathological diagnosis.
Assuntos
Materiais Biocompatíveis/química , Técnicas Biossensoriais , Técnicas Eletroquímicas , Glucose/análise , Peróxido de Hidrogênio/análise , Líquidos Corporais/química , Células Cultivadas , Cobalto/química , Humanos , Hidróxidos/química , Teste de Materiais , Níquel/química , Tamanho da PartículaRESUMO
Electroactive polypyrrole-molybdenum disulfide (MoP) nanocomposites were synthesized and used for modifying screen-printed carbon electrodes (SPCEs) for ultrasensitive detection of berberine, an anticancer drug, in rat plasma. The electroactive nanocomposites were fabricated by exfoliating MoS2 followed by pyrrole polymerization. The effect of polypyrrole in the MoP nanocomposite was evaluated by varying the pyrrole concentration during polymerization, and the resulting nanocomposites prepared with pyrrole concentrations of 10, 20, 30 µL were named as MoP-1, MoP-2, and MoP-3, respectively. The electrochemical characterization of the three MoP nanocomposite sensors revealed that MoP-2/SPCE exhibited the highest electroactivity. The detection of berberine by the three MoP-coated SPCEs revealed that MoP-2/SPCE exhibited the highest activity against berberine due to a two-electron transfer mechanism on the MoP-2/SPCE electrode surface. The detection limit of berberine using the MoP-2/SPCE sensor was found to be about 0.05 µM, which is remarkably lower than the reported detection limits. The interference study proved the selectivity of the MoP-2/SPCE sensor toward berberine in the presence of other bioactive molecules and metal ions. The designed MoP-2/SPCE sensor retained 92% of its initial activity after 15 days of storage at room temperature, with RSD values of about 2.95% and 3.68% for the repeatability and reproducibility studies. Finally, the detection limit of berberine in a rat plasma sample determined using the MoP-2/SPCE sensor was found to be about 5 µM.
Assuntos
Berberina/sangue , Dissulfetos/química , Molibdênio/química , Nanocompostos/química , Polímeros/química , Pirróis/química , Animais , Carbono/química , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Eletrodos , Limite de Detecção , RatosRESUMO
A novel biocomposite film (MWCNTs-PNDGAChi), which contains multiwalled carbon nanotubes (MWCNTs) along with the incorporation of poly(nordihydroguaiaretic acid) and chitosan copolymer (PNDGAChi), has been synthesized on gold electrode by potentiostatic methods. The presence of MWCNTs in the biocomposite film enhances PNDGAChi's surface coverage concentration (Gamma) on the electrode and decreases degradation of PNDGAChi during cycling. The biocomposite film also exhibits promising enhanced electrocatalytic activity toward the oxidation of biochemical compounds such as epinephrine (EP) and norepinephrine (NEP). Cyclic voltammetry was used for the measurement of electroanalytical properties of analytes by means of MWCNTs-PNDGAChi biocomposite film modified gold electrode. The sensitivity values of MWCNTs-PNDGAChi biocomposite film modified gold electrode are higher than the values obtained for PNDGAChi film modified gold electrode. Electrochemical quartz crystal microbalance studies reveal the enhancements in the functional properties of MWCNTs and PNDGAChi present in MWCNTs-PNDGAChi biocomposite film. Surface morphology of the biocomposite films was studied using scanning electron microscopy, atomic force microscopy, and scanning tunneling microscopy. The surface morphology results reveal that PNDGAChi incorporated on MWCNTs. Finally, flow injection analysis was used for the amperometric detection of EP and NEP at MWCNTs-PNDGAChi film modified screen printed carbon electrode.
Assuntos
Eletroquímica/métodos , Epinefrina/metabolismo , Nanotubos de Carbono/química , Norepinefrina/metabolismo , Polímeros/química , Eletrodos , Epinefrina/análise , Norepinefrina/análiseRESUMO
Chitosan-gold collapse gel (CS-Au CG) was prepared by reducing chloroauric acid (HAuCl4) with a polysaccharide, chitosan (CS), in the absence of chemical and physical agents. CS-Au CG was used for the first time as a suitable nano-biocomposite sensing film for efficient one-step electrochemical deposition of poly (bromophenol blue) (PBPB) redox mediator through amino-hydroxyl reaction to prepare a novel anti-androgen drug flutamide (FLU) sensor using glassy carbon electrode (GCE). The effect of electropolymerization cycle, scan rate, pH, and concentration of CS-Au CG/PBPB film on electrochemical behavior of FLU molecules was investigated. The excellent synergetic effect of CS-Au CG/PBPB film showed substantially enhanced electrocatalytic activity for FLU due to the halogen-nitro synthon molecular recognition processes. The selectivity of CS-Au CG/PBPB film sensor for FLU was discussed in detail. The fabricated electrochemical sensor exhibited good linearity in the ranges of 0.01-1245⯵M. And also superior sensitivity (0.63⯵AµM-1â¯cm-2) along with low limit of detection (4.8â¯nM) was obtained for FLU determination. The CS-Au CG/PBPB film showed an excellent selectivity, good reproducibility, and stability. In addition, the proposed sensor was successfully used to analysis of FLU drug in human urine and human blood serum samples with satisfactory results.
Assuntos
Técnicas Biossensoriais , Azul de Bromofenol/química , Quitosana/química , Flutamida/análise , Géis/química , Ouro/química , Oxirredução , Técnicas Eletroquímicas , Flutamida/química , Concentração de Íons de Hidrogênio , Estrutura Molecular , Polimerização , Polímeros , Reprodutibilidade dos Testes , Análise EspectralRESUMO
Development of novel biocompatible sensor material suitable for modest, cost-effective, and rapid practical application is a demanding research interest in the field of electroanalytical chemistry. In this context, for the first time, we utilized biocompatible chitosan-pectin biopolyelectrolyte (CS-PC BPE) complex for the simultaneous electroreduction of an important antibiotic drug (metronidazole-MNZ) and herbicide (metribuzin-MTZ). This sensor reveals an attractive welfares such as simplicity, biocompatibility, and low production cost. Under optimized experimental conditions, the electroanalytical investigation confirmed that CS-PC BPE modified glassy carbon electrode (CS-PC BPE/GCE) was found to sense MNZ and MTZ in the nanomolar range. Moreover, as-prepared CS-PC BPE/GCE exhibited prominent selectivity, stability, and reproducibility. Additionally, the possible MNZ and MTZ sensing mechanism of CS-PC BPE/GCE have been discussed in detail. Lastly, real sample analysis was also carried out and revealed from several investigations that the CS-PC BPE/GCE is a good electrochemical sensor system for the detection of targeted analytes.
Assuntos
Materiais Biocompatíveis/química , Quitosana/química , Metronidazol/sangue , Pectinas/química , Polieletrólitos/química , Triazinas/sangue , Antibacterianos/sangue , Antibacterianos/química , Carbono/química , Quitosana/síntese química , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Eletrodos , Química Verde/métodos , Herbicidas/sangue , Herbicidas/química , Humanos , Limite de Detecção , Metronidazol/química , Peso Molecular , Oxirredução , Pectinas/síntese química , Reprodutibilidade dos Testes , Triazinas/química , ViscosidadeRESUMO
To dates, the facile synthesis of inorganic-coated organic polymer composite has received greater attention in the order of research fields including advanced materials and electrochemical analysis owing to the complementary or synergistic effects. In this context, Pr2O3 and Pr2O3 coated polystyrene (Pr2O3/PS) inorganic-organic colloidal composite were prepared via ultrasound-induced radicals initiated precipitation and dispersion polymerization methods. The synthesized Pr2O3/PS composite was systematically studied by FE-SEM, TEM, EDX, FT-IR, XRD, and XPS analysis. This composite modified glassy carbon electrode (Pr2O3/PS GCE) was utilized to construct a novel electrochemical sensor for the detection assay of chemotherapy agent methotrexate (MTA). Under optimal condition, the designed sensor showed outstanding performance for MTA trace level detection over the linear concentration range of 0.01-236⯵M with a detection limit of 0.8â¯nM for MTA. Furthermore, the prepared sensor accomplished excellent stability and relevant reproducibility, in addition to reliable practical assay in real human blood serum and urine samples. Besides, the possible MTA sensing mechanism of Pr2O3/PS GCE has been deliberated in detail. Our finding suggested that the developed Pr2O3/PS composite might be a favorable material for the fabrication of the high-performance electrochemical sensor.
Assuntos
Eletroquímica/métodos , Metotrexato/análise , Poliestirenos/química , Ondas Ultrassônicas , Eletroquímica/instrumentação , Eletrodos , Transporte de Elétrons , Radicais Livres/química , Humanos , Limite de Detecção , Metotrexato/sangue , Metotrexato/urina , Modelos Moleculares , Conformação Molecular , OxirreduçãoRESUMO
Material combinations of semiconductor with conducting polymer are gaining growing interest due to their enhanced activities in photocatalysis as well as electrochemical sensing. In this present work, we report a facile in situ synthesis of polypyrrole (PPy) polymer-incorporated silver molybdate (Ag2MoO4) nanocomposite that is utilized as a photocatalyst and electrocatalyst for the degradation of pollutant heavy metals, namely, methylene blue (MB) and heavy metal (Cr(VI)), and ciprofloxacin (CIP) and for detection of the drug, azomycin. The synthesized nanocomposite was characterized by various theoretical, spectral, and microscopic studies. Matching of the powder X-ray diffraction pattern with JCPDS no. 76-1747 confirmed the formation of α-Ag2MoO4/PPy. The surface topography and spherical morphology of the nanocomposite were studied using field emission-scanning electron microscopy and transmission electron microscopy. Fourier transform infrared spectral detail expounds the smooth incorporation of PPy to Ag2MoO4. The as-synthesized nanocomposite performs as an efficient photocatalyst in the degradation of MB (99.9%), Cr(VI) (99%), and CIP drug (99.8%) within 10 min. In addition to this, the Ag2MoO4/PPy-modified glassy carbon electrode (GCE) demonstrated excellent electrocatalytic activity in terms of a higher cathodic peak current and lower peak potential when compared with other modified and unmodified GCEs for the detection of azomycin. The Ag2MoO4/PPy/GCE displayed a broader linear response range and lower detection limit of 0.5-499 µM and 65 nM, respectively. Moreover, other potentially co-interfering compounds, such as a similar functional group-containing biological substances and inorganic species, have no interference effect toward azomycin sensing.
Assuntos
Poluentes Ambientais/química , Molibdênio/química , Nanocompostos/química , Polímeros/química , Pirróis/química , Prata/química , Catálise , Ciprofloxacina/química , Azul de Metileno/química , Nitroimidazóis/químicaRESUMO
Well-defined CoS nanorods (NR) were synthesized using a simple hydrothermal method, and were tested as an electrode material for electro-oxidation of vanillin. The NR material was characterized with regard to morphology, crystallinity, and electro-activity by use of appropriate analytical techniques. The resulting CoS NR@Nafion modified glassy carbon electrode (GCE) exhibited efficient electro-oxidation of vanillin with a considerable linear range of current-vs-concentration (0.5-56µM vanillin) and a detection limit of 0.07µM. Also, food samples containing vanillin were studied to test suitability for commercial applications.
Assuntos
Antioxidantes/análise , Benzaldeídos/análise , Chocolate/análise , Cobalto/química , Técnicas Eletroquímicas/métodos , Nanotubos/química , Eletrodos , Polímeros de Fluorcarboneto/química , Análise de Alimentos , Limite de Detecção , Nanotubos/ultraestrutura , OxirreduçãoRESUMO
We described the synthesis of biscuit-like copper oxide (CuO) by the precipitation cum thermal annealing process. The biscuit-like CuO microstructures were successfully obtained by template free synthesis process. Thereby, the oxalic acid was used as the shape forming agent. Herein, the role of the sonic wave was quite important to controlling the shape. The CuO microstructures were characterized by the X-ray diffraction pattern, scanning electron microscope and energy dispersive X-ray analysis. The as-prepared CuO was used to fabricate the disposable sensor electrode using screen printed carbon electrode (SPCE). The CuO modified SPCE was successfully determined the glucose with the linear concentration ranging from 0.0005 to 4.03mM and the lowest detection limit of 0.1µM. The biscuit-like CuO microstructures based glucose sensor displayed appreciable analytical performance than the other CuO nanostructures. Moreover, the disposable CuO/SPCE was applied to determine the glucose in human blood serum, saliva and urine samples. The developed glucose sensor attained good recoveries in real sample analysis, hence, it is applicable for the commercial applications.
Assuntos
Cobre/química , Glucose/análise , Glicemia/análise , Eletrodos , Humanos , Limite de Detecção , Nanoestruturas/química , Ácido Oxálico/química , Saliva/química , Urina/químicaRESUMO
To date, the natural alkaloids are mostly used in the field of pharmacological applications and the active substance of palmatine was extensively used in cancer therapy and other biomedical applications. Hence, in this study we report a simple preparation of poly-l-lysine (PLL) electro-polymerized on the surface of functionalized multiwalled carbon nanotubes (f-MWCNT) for electrochemical detection of palmatine content in human serum and urine samples. The active amino group of PLL plays a vital role towards the oxidation palmatine and exhibits superior electrocatalytic activity. Under optimum conditions, the prepared f-MWCNT/PLL composite shows a wide linear response range over the palmatine concentration ranging from 0.5µM to 425µM, and a detection limit (LOD) of 0.12µM based on S/N =3 (signal to noise ratio). The real time monitoring of palmatine content in serum and urine samples displays an appropriate recoveries and excellent performance for the practical analysis. The advantage of this developed system was simple, higher electrocatalytic activity, long-term stability and low cost. We hope that the prepared composite opens a new way for the fabrication of different biosensors in the field of biomedical application.
Assuntos
Alcaloides de Berberina/sangue , Alcaloides de Berberina/urina , Nanotubos de Carbono/química , Polilisina/química , Materiais Biocompatíveis/química , Técnicas Biossensoriais/métodos , Catálise , Técnicas Eletroquímicas , Eletrodos , Humanos , Limite de Detecção , Microscopia Eletrônica de Varredura , Nanocompostos/química , Oxirredução , Tamanho da Partícula , Espectroscopia Fotoeletrônica , Polimerização , Espectroscopia de Infravermelho com Transformada de Fourier , Propriedades de SuperfícieRESUMO
A simple and cost effective synthesis of nanomaterials with advanced physical and chemical properties have received much attention to the researchers, and is of interest to the researchers from different disciplines. In the present work, we report a simple and one pot electrochemical synthesis of poly(melamine) entrapped gold nanoparticles (PM-AuNPs) composite. The PM-AuNPs composite was prepared by a single step electrochemical method, wherein the AuNPs and PM were simultaneously fabricated on the electrode surface. The as-prepared materials were characterized by various physicochemical methods. The PM-AuNPs composite modified electrode was used as an electrocatalyst for oxidation of catechol (CC) due to its well-defined redox behavior and enhanced electro-oxidation ability towards CC than other modified electrodes. Under optimized conditions, the differential pulse voltammetry (DPV) was used for the determination of CC. The DPV response of CC was linear over the concentration ranging from 0.5 to 175.5µM with a detection limit of 0.011µM. The PM-AuNPs composite modified electrode exhibits the high selectivity in the presence of range of potentially interfering compounds including dihydroxybenzene isomers. The sensor shows excellent practicality in CC containing water samples, which reveals the potential ability of PM-AuNPs composite modified electrode towards the determination of CC in real samples.