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1.
Anal Methods ; 16(33): 5676-5683, 2024 Aug 22.
Article in English | MEDLINE | ID: mdl-39118596

ABSTRACT

In this study, we describe a rapid and high-throughput smartphone-based digital colorimetric method for determining urea in milk. A compact and cost-effective 3D-printed image box microplate-based system was designed to measure multiple samples simultaneously, using minimal sample and reagent volumes. The apparatus was applied for the quantification of urea in milk based on its reaction with p-dimethylaminobenzaldehyde (DMAB). The predictive performance of calibration was evaluated using RGB and different colour models (CMYK, HSV, and CIELAB), with the average blue (B) values of the RGB selected as the analytical signal for urea quantification. Under optimized conditions, a urea concentration linear range from 50 to 400 mg L-1 was observed, with a limit of detection (LOD) of 15 mg L-1. The values found with the smartphone-based DIC procedure are in good agreement with spectrophotometric (spectrophotometer and microplate treader) and reference method (mid-infrared spectroscopy) values. This proposed approach offers an accessible and efficient solution for digital image colorimetry, with potential applications for various target analytes in milk and other fields requiring high-throughput colorimetric analysis.


Subject(s)
Colorimetry , Milk , Printing, Three-Dimensional , Smartphone , Urea , Milk/chemistry , Colorimetry/methods , Colorimetry/instrumentation , Animals , Urea/analysis , Urea/chemistry , Limit of Detection , Benzaldehydes/chemistry , Benzaldehydes/analysis
2.
Mikrochim Acta ; 191(7): 425, 2024 06 27.
Article in English | MEDLINE | ID: mdl-38926184

ABSTRACT

A solvothermal synthesis of ultrasmall cerium oxide nanoparticles (USCeOxNPs) with an average size of 0.73 ± 0.07 nm using deep eutectic solvent (DES) as a stabilizing medium at a temperature of 90 ºC is reported. Transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) were used to morphologically characterize the USCeOxNPs. These revealed approximately spherical shapes with emission lines characteristic of cerium. Selected area electron diffraction (SAED) was used to determine the crystalline structure of the cerium oxide nanoparticles (CeO2NPs), revealing the presence of crystalline cubic structures. The USCeOxNPs-DES/CB film was characterized by scanning electron microscopy (SEM), which demonstrated the spherical characteristic of CB with layers slightly covered by DES residues. DES was characterized by Fourier transform infrared (FT-IR) and nuclear magnetic resonance (NMR), indicating its formation through hydrogen bonds between the precursors. An electrochemical sensor for dopamine (DA) determination in biological fluids was developed using the USCeOxNPs together with carbon black (CB). An enhanced current response was observed on DA voltammetric determination, and this can be attributed to the USCeOxNPs. This sensor displayed linear responses for DA in the range 5.0 × 10-7 mol L-1 to 3.2 × 10-4 mol L-1, with a limit of detection of 80 nmol L-1. Besides detectability, excellent performances were verified for repeatability and anti-interference. The sensor based on USCeOxNPs synthesized in DES in a simpler and environmentally friendly way was successfully applied to determine DA in biological matrix.


Subject(s)
Cerium , Dopamine , Electrochemical Techniques , Cerium/chemistry , Dopamine/analysis , Dopamine/blood , Electrochemical Techniques/methods , Humans , Deep Eutectic Solvents/chemistry , Nanoparticles/chemistry , Limit of Detection , Metal Nanoparticles/chemistry , Particle Size
3.
Mikrochim Acta ; 191(7): 375, 2024 Jun 07.
Article in English | MEDLINE | ID: mdl-38849611

ABSTRACT

The production, optimisation, physicochemical, and electroanalytical characterisation of a low-cost electrically conductive additive manufacturing filament made with recycled poly(lactic acid) (rPLA), castor oil, carbon black, and graphite (CB-G/PLA) is reported. Through optimising the carbon black and graphite loading, the best ratio for conductivity, low material cost, and printability was found to be 60% carbon black to 40% graphite. The maximum composition within the rPLA with 10 wt% castor oil was found to be an overall nanocarbon loading of 35 wt% which produced a price of less than £0.01 per electrode whilst still offering excellent low-temperature flexibility and reproducible printing. The additive manufactured electrodes produced from this filament offered excellent electrochemical performance, with a heterogeneous electron (charge) transfer rate constant, k0 calculated to be (2.6 ± 0.1) × 10-3 cm s-1 compared to (0.46 ± 0.03) × 10-3 cm s-1 for the commercial PLA benchmark. The additive manufactured electrodes were applied to the determination of ß-estradiol, achieving a sensitivity of 400 nA µM-1, a limit of quantification of 70 nM, and a limit of detection of 21 nM, which compared excellently to other reports in the literature. The system was then applied to the detection of ß-estradiol within four real water samples, including tap, bottled, river, and lake water, where recoveries between 95 and 109% were obtained. Due to the ability to create high-performance filament at a low material cost (£0.06 per gram) and through the use of more sustainable materials such as recycled polymers, bio-based plasticisers, and naturally occurring graphite, additive manufacturing will have a permanent place within the electroanalysis arsenal in the future.

4.
Biosensors (Basel) ; 13(7)2023 Jun 29.
Article in English | MEDLINE | ID: mdl-37504089

ABSTRACT

The present study reports the development and application of a flow injection analysis (FIA) system for the simultaneous determination of uric acid (UA) and caffeine (CAF) using cathodically pretreated boron-doped diamond electrode (CPT-BDD) and multiple-pulse amperometry (MPA). The electrochemical profiles of UA and CAF were analyzed via cyclic voltammetry in the potential range of 0.20-1.7 V using 0.10 mol L-1 H2SO4 solution as supporting electrolyte. Under optimized conditions, two oxidation peaks at potentials of 0.80 V (UA) and 1.4 V (CAF) were observed; the application of these potentials using multiple-pulse amperometry yielded concentration linear ranges of 5.0 × 10-8-2.2 × 10-5 mol L-1 (UA) and 5.0 × 10-8-1.9 × 10-5 mol L-1 (CAF) and limits of detection of 1.1 × 10-8 and 1.3 × 10-8 mol L-1 for UA and CAF, respectively. The proposed method exhibited good repeatability and stability, and no interference was detected in the electrochemical signals of UA and CAF in the presence of glucose, NaCl, KH2PO4, CaCl2, urea, Pb, Ni, and Cd. The application of the FIA-MPA method for the analysis of environmental samples resulted in recovery rates ranging between 98 and 104%. The results obtained showed that the BDD sensor exhibited a good analytical performance when applied for CAF and UA determination, especially when compared to other sensors reported in the literature.


Subject(s)
Caffeine , Uric Acid , Caffeine/analysis , Oxidation-Reduction , Electrodes , Electrochemical Techniques/methods
5.
Biosensors (Basel) ; 13(3)2023 Mar 13.
Article in English | MEDLINE | ID: mdl-36979591

ABSTRACT

A sensitive and selective label-free photoelectrochemical (PEC) immunosensor was designed for the detection of cardiac troponin I (cTnI). The platform was based on a fluorine-doped tin oxide (FTO)-coated glass photoelectrode modified with bismuth vanadate (BiVO4) and sensitized by an electrodeposited bismuth sulfide (Bi2S3) film. The PEC response of the Bi2S3/BiVO4/FTO platform for the ascorbic acid (AA) donor molecule was approximately 1.6-fold higher than the response observed in the absence of Bi2S3. The cTnI antibodies (anti-cTnI) were immobilized on the Bi2S3/BiVO4/FTO platform surface to produce the anti-cTnI/Bi2S3/BiVO4/FTO immunosensor, which was incubated in cTnI solution to inhibit the AA photocurrent. The photocurrent obtained by the proposed immunosensor presented a linear relationship with the logarithm of the cTnI concentration, ranging from 1 pg mL-1 to 1000 ng mL-1. The immunosensor was successfully employed in artificial blood plasma samples for the detection of cTnI, with recovery values ranging from 98.0% to 98.5%.


Subject(s)
Biosensing Techniques , Myocardial Infarction , Humans , Limit of Detection , Electrochemical Techniques , Troponin I , Fluorine , Immunoassay , Electrodes , Myocardial Infarction/diagnosis , Biomarkers
6.
Anal Methods ; 15(8): 1077-1086, 2023 Feb 23.
Article in English | MEDLINE | ID: mdl-36752550

ABSTRACT

The versatility of chitosan (Ch) biopolymer as a metallic nanoparticle stabilizing agent and excellent former of thin films on glassy carbon was explored in this work for the sustainable manufacture of novel electrochemical sensors based on carbon black (CB) and chitosan-stabilized platinum nanoparticles (Ch-PtNPs). Platinum nanoparticles highly stabilized by chitosan were easily synthesized at room temperature and characterized by HR-TEM, UV-vis, and voltammetry. Ch-PtNPs presented an average diameter of 2.7 nm, and typical voltammetric peaks of Pt in sulfuric acid medium were detected for films containing Ch-PtNPs. As a proof of concept, the CB-Ch-PtNP electrode was applied in the determination of hydrogen peroxide (H2O2) and the endocrine disruptor bisphenol A (BPA). Pronounced electrocatalytic activity towards H2O2 reduction was observed in the presence of Ch-PtNPs in the films, guaranteeing the non-enzymatic determination of H2O2 by chronoamperometry, with a limit of detection of 10 µmol L-1. In the determination of BPA by differential pulse adsorptive anodic stripping voltammetry (DPAdASV), under optimal experimental conditions, a wide linear response range and a limit of detection at the nanomolar level (7.9 nmol L-1) were achieved. In addition, excellent repeatabilities of sensor response and sensor fabrication, and accuracy in the analysis of natural water samples were obtained.

7.
J Pharm Biomed Anal ; 221: 115032, 2022 Nov 30.
Article in English | MEDLINE | ID: mdl-36152488

ABSTRACT

The outstanding electronic properties of carbon black (CB) and its economic advantages have fueled its application as nanostructured electrode material for the development of new electrochemical sensors and biosensors. CB-based electrochemical sensing devices have been found to exhibit high surface area, fast charge transfer kinetics, and excellent functionalization. In the present work, we set forth a comprehensive review of the recent advances made in the development and application of CB-based electrochemical devices for pharmaceutical and biomedical analyses - from quantitative monitoring of drug formulations to clinical diagnoses - and the underlying challenges and constraints that need to be overcome. We also present a thorough discussion about the strategies and techniques employed in the development of new electrochemical sensing platforms and in the enhancement of their analytical properties and biocompatibility for anchoring active biomolecules, as well as the combination of these sensing devices with other materials aiming at boosting the performance and efficiency of the sensors.


Subject(s)
Biosensing Techniques , Nanostructures , Biosensing Techniques/methods , Electrochemical Techniques/methods , Nanostructures/chemistry , Pharmaceutical Preparations , Soot
8.
Anal Methods ; 14(39): 3859-3866, 2022 10 13.
Article in English | MEDLINE | ID: mdl-36129055

ABSTRACT

A new electrode was prepared based on functionalized graphene and gold nanoparticles dispersed in a chitosan film. Such an electrochemical sensor determines ofloxacin in the presence of dopamine, paracetamol, and caffeine. Characterization (morphological and electrochemical) was done using scanning electron microscopy, electrochemical impedance spectroscopy, and cyclic voltammetry. The sensor design improved the analytical signal, the electrochemical activity, and the electron transfer rate. Ofloxacin was determined by square-wave voltammetry, with a linear concentration range of 0.10-4.9 µmol L-1 (r = 0.999, LOD = 12 nmol L-1). The proposed sensor showed good repeatability and selectivity and was applied successfully to the determination of ofloxacin in pharmaceutical formulations, synthetic urine, and water river samples. The proposed method proved to be excellent; therefore, it is an alternative method for the determination of ofloxacin.


Subject(s)
Chitosan , Graphite , Metal Nanoparticles , Acetaminophen , Caffeine/chemistry , Carbon/chemistry , Dopamine , Electrodes , Gold/chemistry , Graphite/chemistry , Metal Nanoparticles/chemistry , Ofloxacin , Pharmaceutical Preparations , Water
9.
Anal Methods ; 14(20): 2003-2013, 2022 05 27.
Article in English | MEDLINE | ID: mdl-35543344

ABSTRACT

The present study reports the synthesis and characterization of hydrophobic deep eutectic solvents (HDES) based on fatty acids and tetrabutylammonium bromide (TBAB) or 1-octanol using Fourier transform infrared spectroscopy, and the analysis of the physicochemical properties (viscosity, density, electrical conductivity, and water content) of these solvents. A carbon paste electrode modified with 6.0% (m/m) decanoic acid and TBAB-based HDES was characterized by cyclic voltammetry, electrochemical impedance spectroscopy, and scanning electron microscopy. The oxidation peak currents of the proposed electrode were enhanced by its high electrochemical activity, fast electron transfer rate, and high surface area, while a remarkable decrease was observed in the peak potential separation. The electrochemical determination of hydroquinone (H2Q) was carried out using square-wave adsorptive anodic stripping voltammetry (SWAdASV). The electrode response was found to be linear in the H2Q concentration range of 2.5 × 10-6-3.0 × 10-3 mol L-1, with the limit of detection (LOD) of 7.7 × 10-7 mol L-1. The method was successfully applied for H2Q determination in dermatological creams.


Subject(s)
Carbon , Hydroquinones , Carbon/chemistry , Deep Eutectic Solvents , Electrochemical Techniques/methods , Electrodes , Hydroquinones/analysis , Solvents
10.
Talanta ; 236: 122881, 2022 Jan 01.
Article in English | MEDLINE | ID: mdl-34635261

ABSTRACT

For the first time carbon black based electrode modified with paraffin was applied as a sensor on voltammetry of immobilized microparticles (VIMP) approach for determination of lead solid residues in hair dye samples. The solid microparticles of Pb(II) (Pb(CH3COO)2(s)) immobilized into the carbon paste sensor containing carbon black and paraffin were firstly reduced at initial potentials and further reoxidized at around -0.60 V during anodic scan. Electroanalytical parameters as well as supporting electrolyte composition, and pH were also evaluated. An analytical curve in 0.2 mol L-1 phosphate buffer solution (pH 5.0) from 0.04 to 3.2 µg (R2 = 0.999) with detection and quantification limits of 4 and 13 ng, respectively, were achieved. The method was applied to quantify lead solid residues in hair dye samples without previous mineralization or complex sample pre-treatment. Besides adequate repeatability, stability and selectivity of the developed sensor based on VIMP features, the method using carbon black based sensor was considered advantageous comparing to the results recorded by a spectrometric method (relative error lower than 8%) from several analytical viewpoints.


Subject(s)
Soot , Electrodes
11.
Anal Methods ; 13(38): 4495-4502, 2021 10 08.
Article in English | MEDLINE | ID: mdl-34514492

ABSTRACT

A modified glassy carbon electrode with carbon black (CB) and gold nanoparticles (AuNPs) within a crosslinked chitosan (CTS) film is proposed in this work. The electroanalytical performance of the modified CB-CTS-AuNPs/GCE has been evaluated towards the voltammetric sensing of ketoconazole (KTO), a widespread antifungal drug. The nanocomposite was characterized by scanning electron microscopy, X-ray diffraction spectroscopy, and electrochemistry experiments. The evaluation of the electrochemical behaviour of KTO on the proposed modified electrode shows an irreversible oxidation process at a potential of +0.65 V (vs. Ag/AgCl (3.0 mol L-1 KCl)). This redox process was explored to carry out KTO sensing using square-wave voltammetry. The analytical curve was linear in the KTO concentration range from 0.10 to 2.9 µmol L-1, with a limit of detection (LOD) of 4.4 nmol L-1 and a sensitivity of 3.6 µA L µmol-1. This modified electrode was successfully applied to the determination of KTO in pharmaceutical formulations and biological fluid samples.


Subject(s)
Chitosan , Metal Nanoparticles , Nanocomposites , Gold , Ketoconazole , Soot
12.
Talanta ; 224: 121804, 2021 Mar 01.
Article in English | MEDLINE | ID: mdl-33379030

ABSTRACT

The present work reports the development of a sensitive and selective method for ethinylestradiol detection using screen-printed electrode (SPE) modified with functionalized graphene (FG), graphene quantum dots (GQDs) and magnetic nanoparticles coated with molecularly imprinted polymers (mag@MIP). The performance of the mag@MIP sensor was compared with that of a non-molecularly imprinted sensor (mag@NIP). Chemical and physical characterizations of the mag@NIP and mag@MIP sensors were performed using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and Brunauer-Emmett-Teller (BET) techniques. The electrochemical behavior of the electrodes investigated, which included (mag@MIP)-GQDs-FG-NF/SPE, (mag@NIP)-GQDs-FG-NF/SPE, GQDs-FG-NF/SPE and FG-NF/SPE, was evaluated by cyclic voltammetry. The results obtained show a significant increase in peak current magnitude for (mag@MIP)-GQDs-FG-NF/SPE. Using square wave voltammetry experiments, the efficiency of the (mag@MIP)-GQDs-FG-NF/SPE sensor was also tested under optimized conditions. The linear response range obtained for ethinylestradiol concentration was 10 nmol L-1 to 2.5 µmol L-1, with limit of detection of 2.6 nmol L-1. The analytical signal of the (mag@MIP)-GQDs-FG-NF/SPE sensor suffered no interference from different compounds and the sensor exhibited good repeatability. The proposed sensor was successfully applied for ethynilestradiol detection in river water, serum and urine samples, where recovery rates between 96 to 105% and 97-104% were obtained for environmental and biological samples, respectively.


Subject(s)
Graphite , Magnetite Nanoparticles , Molecular Imprinting , Quantum Dots , Electrochemical Techniques , Electrodes , Ethinyl Estradiol , Limit of Detection , Molecularly Imprinted Polymers
13.
Talanta ; 222: 121539, 2021 Jan 15.
Article in English | MEDLINE | ID: mdl-33167247

ABSTRACT

The present study reports the development of graphite pencil electrode modified with palladium nanoparticles (PdNPs) and its application as an electrochemical sensor for the simultaneous detection of direct yellow 50, tryptophan, carbendazim and caffeine in river water and synthetic urine samples. The combination involving the conductive surface of the graphite pencil electrode (GPE) and the enlargement of the surface area caused by the use of palladium nanoparticles (PdNPs) led to the improvement of the analytical performance of the proposed device. The surface of the GPE-PdNPs was characterized by scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The charge transfer kinetics of the electrode was evaluated based on the electrochemical analysis of the potassium ferricyanide redox probe. Using square wave voltammetry (SWV), well-defined and fully resolved anodic peaks were detected for the analytes, with peak-to-peak potential separation not less than 200 mV. Under optimised conditions, the following linear range concentrations were obtained: 0.99-9.9 µmol L-1 for direct yellow 50; 1.2-12 µmol L-1 for tryptophan; 0.20-1.6 µmol L-1 for carbendazim; and 25-190 µmol L-1 for caffeine. The sensor showed good sensitivity, repeatability, and stability. The device was successfully applied for the determination of analytes in urine and river water samples, where recovery rates close to 100% were obtained. Due to its low cost and reusability by simple polishing, the sensor has strong potential to be used as an electrochemical sensor for the determination of different analytes.


Subject(s)
Graphite , Metal Nanoparticles , Azo Compounds , Benzimidazoles , Caffeine , Carbamates , Electrochemical Techniques , Electrodes , Naphthalenes , Palladium , Tryptophan
14.
Anal Chim Acta ; 1139: 198-221, 2020 Dec 01.
Article in English | MEDLINE | ID: mdl-33190704

ABSTRACT

The detection of phenolic compounds is relevant not only for their possible benefits to human health but also for their role as chemical pollutants, including as endocrine disruptors. The required monitoring of such compounds on-site or in field analysis can be performed with electrochemical biosensors made with polyphenol oxidases (PPO). In this review, we describe biosensors containing the oxidases tyrosinase and laccase, in addition to crude extracts and tissues from plants as enzyme sources. From the survey in the literature, we found that significant advances to obtain sensitive, robust biosensors arise from the synergy reached with a diversity of nanomaterials employed in the matrix. These nanomaterials are mostly metallic nanoparticles and carbon nanostructures, which offer a suitable environment to preserve the activity of the enzymes and enhance electron transport. Besides presenting a summary of contributions to electrochemical biosensors containing PPOs in the last five years, we discuss the trends and challenges to take these biosensors to the market, especially for biomedical applications.


Subject(s)
Biosensing Techniques , Monophenol Monooxygenase , Nanostructures , Carbon , Electrochemical Techniques , Laccase
15.
Materials (Basel) ; 13(6)2020 Mar 14.
Article in English | MEDLINE | ID: mdl-32183300

ABSTRACT

The present work reports the degradation of 4-nitrophenol using BiVO4/CuO hybrid material synthesized by the precipitation of BiVO4 in the presence of CuO. Morphological and structural characterizations were performed using X-ray diffraction and scanning electronic microscopy coupled to energy dispersive X-ray spectroscopy. Through the calculation of the Kubelka-Munk function applied to diffuse reflectance spectrophotometry data, the hybrid material presented absorption edge of 1.85 eV. The formation of p-n heterojunction between BiVO4 and CuO renders the hybrid material suitable for the construction of a photoanode employed in hydroxyl radical generation. UV-vis spectrophotometry and high-performance liquid chromatography experiments were performed in order to monitor the degradation of 4-nitrophenol and the formation of secondary products. Additional information regarding the hybrid material was obtained through ion chromatography and total organic carbon analyses. The application of BiVO4/CuO-based photocatalyzer led to a 50.2% decrease in total organic carbon after the degradation of 4-nitrophenol. Based on the results obtained in the study, BiVO4/CuO has proved to be a promising material suitable for the removal of recalcitrant compounds in water treatment plants.

16.
Talanta ; 209: 120588, 2020 Mar 01.
Article in English | MEDLINE | ID: mdl-31891996

ABSTRACT

The ionic liquid (IL) 1-butyl-3-methylimidazolium tetrafluoroborate and carbon black (CB) nanoparticles were incorporated within a crosslinked chitosan film over the surface of a glassy carbon electrode, and the obtained architecture explored to the sensitive voltammetric sensing of Allura red colorant in soft drinking powders. The different electrodic surfaces were morphologically and electrochemically characterized. From the modification of glassy carbon electrode with IL and CB, a significantly enhanced voltammetric response was achieved toward the Allura red irreversible oxidation reaction. The type and amount of IL employed in the electrode modification step as well as all the others experimental parameters affecting the sensor response by square-wave adsorptive anodic stripping voltammetry (SWAdASV) were systematically optimized. Under the optimum experimental conditions, the proposed SWAdASV procedure provided a linear analytical curve in the concentration range of 3.98 × 10-8 to 9.09 × 10-7 mol L-1 and a low limit of detection of 9.1 × 10-10 mol L-1 (0.91 nmol L-1). The proposed sensor presented good precision and no matrice effects as shown from repeatability tests, concomitant studies and addition/recovery assays. The developed SWAdASV procedure was applied successfully in the determination of Allura red content in commercial soft drink powder samples, and the results were in close agreement with those obtained using a comparative spectrophotometric method at a confidence level of 95%.

17.
Talanta ; 206: 120252, 2020 Jan 01.
Article in English | MEDLINE | ID: mdl-31514822

ABSTRACT

A new electrochemical device based on a combination of nanomaterials such as Printex 6L Carbon and cadmium telluride quantum dots within a poly(3,4-ethylenedioxythiophene) polystyrene sulfonate film was developed for sensitive determination of amoxicillin. The morphological, structural and electrochemical characteristics of the nanostructured material were evaluated using X-ray diffraction, confocal microscopy, transmission electron microscopy and voltammetric techniques. The synergy between these materials increased the electrochemical activity, the electron transfer rate and the electrode surface area, leading to a high magnitude of the anodic peak current for the determination of amoxicillin. The electrochemical determination of the antibiotic was carried out using square-wave voltammetry. Under the optimised experimental conditions, the proposed sensor showed high sensitivity, repeatability and stability to amoxicillin determination, with an analytical curve in the amoxicillin concentration range from 0.90 to 69 µmol L-1, and a low detection limit of 50 nmol L-1. No significant interference in the electrochemical signal of amoxicillin was observed from potential biological interferences and drugs widely used, such as uric acid, paracetamol, urea, ascorbic acid and caffeine. It was demonstrated that without any sample pre-treatment and using a simple measurement device, the sensor could be an alternative method for not only the analysis of pharmaceutical products (commercial tablets) and clinical samples (urine), but also to examine food quality (milk samples).


Subject(s)
Amoxicillin/analysis , Anti-Bacterial Agents/analysis , Quantum Dots/chemistry , Amoxicillin/urine , Animals , Anti-Bacterial Agents/urine , Bridged Bicyclo Compounds, Heterocyclic/chemistry , Cadmium Compounds/chemistry , Carbon/chemistry , Electrochemical Techniques/instrumentation , Electrochemical Techniques/methods , Electrodes , Food Contamination/analysis , Limit of Detection , Milk/chemistry , Polymers/chemistry , Polystyrenes/chemistry , Tellurium/chemistry
18.
Talanta ; 207: 120277, 2020 Jan 15.
Article in English | MEDLINE | ID: mdl-31594622

ABSTRACT

A low-cost and disposable microcell was constructed with a screen-printed electrode for the non-enzymatic electrochemical determination of creatinine. The working electrode was modified with carbon black and maintained in contact with paper-adsorbed iron (III) ions. A small sample volume of 3 µL was required for the device operation. Then, iron (III) ions were complexed in the presence of creatinine in a chemical step, followed by an electrochemical reduction of non-complexed metallic ions in excess. Cyclic voltammetry and differential-pulse voltammetry experiments were employed for the electrochemical characterizations and analytical performance evaluation of the microcell. The working electrode modification with carbon black provided a significant increase of analytical signal. The sensor presented a linear response for creatinine concentrations ranging from 0.10 to 6.5 mmol L-1, with a limit of detection of 0.043 mmol L-1. Experiments for creatinine determination in real samples were successful performed through of standard recovery in urine.


Subject(s)
Creatinine/analysis , Electrochemistry/instrumentation , Microarray Analysis/instrumentation , Printing , Creatinine/chemistry , Creatinine/urine , Electrodes , Green Chemistry Technology , Humans , Iron/chemistry , Limit of Detection , Soot/chemistry
19.
Talanta ; 203: 280-286, 2019 Oct 01.
Article in English | MEDLINE | ID: mdl-31202339

ABSTRACT

A disposable microfluidic electrochemical paper-based device for multiplexed analysis based on sixteen independent microfluidic channels with electrochemical detection is proposed. A major advantage of this work was the non-necessary use of a wax printer for devices manufacturing which has a high cost of operation. In addition, a commercial multiplexing module was used that has the multiplexing capability of 8-16 channels and, for the first time using this module, the strategy of multiplexing both the working and reference electrodes were used. These sixteen channels with the respective sensors can be operated employing one or multiple electrochemical techniques with good repeatability and reproducibility for high throughput analysis. As a proof of concept, the electrochemical performance of device was tested with ferrocenecarboxylic acid solution employing cyclic voltammetry, square-wave voltammetry, differential-pulse voltammetry and chronoamperometry. This innovative sensing platform presented capacity of production in large scale and application for clinical tests with safety and short time of assays. A biosensor was constructed using glucose oxidase on the platform for the glucose determination in urine as a non-invasive strategy. The analytical curve was linear in the glucose concentration range from 1.0 × 10-4 mol L-1 to 4 × 10-2 mol L-1, with a limit of detection of 3 × 10-5 mol L-1.

20.
Mater Sci Eng C Mater Biol Appl ; 99: 1415-1423, 2019 Jun.
Article in English | MEDLINE | ID: mdl-30889677

ABSTRACT

A composite electrode based on graphite oxide (GrO)-polyurethane (PU) modified with ß-cyclodextrin (CD) was proposed for the simultaneous determination of three drugs: terbutaline (TER), nimesulide (NIM), and methocarbamol (MET), as possible contaminants in river water samples. To evaluate the performance of the proposed CD-GrOPUE, voltammetric techniques were used and two other electrodes were fabricated (GrOPUE and GrPUE) for comparison. The functionalization of the GrO was confirmed by scanning electron microscopy images, energy-dispersive X-ray spectroscopy analysis, and thermogravimetry. Cyclic voltammograms obtained for TER, NIM, and MET indicated an irreversible behaviour at 0.6 V, 0.9 V and 1.2 V (vs. Ag/AgCl (3 mol L-1 KCl)), respectively, on each working electrode, with the highest peak current values been obtained using the CD-GrOPUE. Under optimal conditions, using square-wave voltammetry, the linear ranges obtained (and limit of detection) for TER, NIM, and MET were 2.5-30 (0.55), 0.62-7.3 (0.083), and 0.62-7.3 (0.077) µmol L-1, respectively. The analytical method developed were applied in the simultaneous determination of TER, NIM, and MET in river water samples, with results like those obtained using a reference spectrophotometric method (at a confidence level of 95%). One can conclude, that the modification of GrO with CD arrays made possible the development of a robust and simple sensor platform for environmental analyses.


Subject(s)
Environmental Pollutants/analysis , Graphite/chemistry , Polyurethanes/chemistry , beta-Cyclodextrins/chemistry , Electrochemical Techniques , Electrodes , Reproducibility of Results , Rivers/chemistry , Thermogravimetry , Water Pollutants, Chemical/analysis
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