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1.
Mikrochim Acta ; 191(2): 96, 2024 01 15.
Artigo em Inglês | MEDLINE | ID: mdl-38225436

RESUMO

The combination of multi-walled carbon nanotubes (MWCNT) and carbon black (CB) is presented to produce a high-performance electrically conductive recycled additive manufacturing filament. The filament and subsequent additively manufactured electrodes were characterised by TGA, XPS, Raman, and SEM and showed excellent low-temperature flexibility. The MWCNT/CB filament exhibited an improved electrochemical performance compared to an identical in-house produced bespoke filament using only CB. A heterogeneous electrochemical rate constant, [Formula: see text] of 1.71 (± 0.19) × 10-3 cm s-1 was obtained, showing an almost six times improvement over the commonly used commercial conductive CB/PLA. The filament was successfully tested for the simultaneous determination of acetaminophen and phenylephrine, producing linear ranges of 5-60 and 5-200 µM, sensitivities of 0.05 µA µM-1 and 0.14 µA µM-1, and limits of detection of 0.04 µM and 0.38 µM, respectively. A print-at-home device is presented where a removable lid comprised of rPLA can be placed onto a drinking vessel and the working, counter, and reference components made from our bespoke MWCNT/CB filament. The print-at-home device was successfully used to determine both compounds within real pharmaceutical products, with recoveries between 87 and 120% over a range of three real samples. This work paves the way for fabricating new highly conductive filaments using a combination of carbon materials with different morphologies and physicochemical properties and their application to produce additively manufactured electrodes with greatly improved electrochemical performance.


Assuntos
Acetaminofen , Nanotubos de Carbono , Acetaminofen/análise , Nanotubos de Carbono/química , Fuligem , Fenilefrina , Técnicas Eletroquímicas
2.
Lab Chip ; 24(3): 467-479, 2024 Jan 30.
Artigo em Inglês | MEDLINE | ID: mdl-38126917

RESUMO

Multiple protocols have been reported to fabricate paper-based analytical devices (PADs). However, some of these techniques must be revised because of the instrumentation required. This paper describes a versatile and globally affordable method to fabricate PADs using office paper as a substrate and a laser printing technique to define hydrophobic barriers on paper surfaces. To demonstrate the feasibility of the alternatives proposed in this study, the fabrication of devices for three types of detection commonly associated with using PADs was demonstrated: colorimetric detection, electrochemical detection, and mass spectrometry associated with a paper-spray ionization (PSI-MS) technique. Besides that, an evaluation of the type of paper used and chemical modifications required on the substrate surface are also presented in this report. Overall, the developed protocol was suitable for using office paper as a substrate, and the laser printing technique as an efficient fabrication method when using this substrate is accessible at a resource-limited point-of-need. Target analytes were used as a proof of concept for these detection techniques. Colorimetric detection was carried out for acetaminophen, iron, nitrate, and nitrite with limits of detection of 0.04 µg, 4.5 mg mL-1, 2.7 µmol L-1, and 6.8 µmol L-1, respectively. A limit of detection of 0.048 fg mL-1 was obtained for the electrochemical analysis of prostate-specific antigen. Colorimetric and electrochemical devices revealed satisfactory performance when office paper with a grammage of 90 g m-2 was employed. Methyldopa analysis was also carried out using PSI-MS, which showed a good response in the same paper weight and behavior compared to chromatographic paper.

3.
ACS Appl Mater Interfaces ; 15(48): 56424-56432, 2023 Dec 06.
Artigo em Inglês | MEDLINE | ID: mdl-37982226

RESUMO

The concentration of environmental pollutants needs to be monitored constantly by reliable analytical methods since they pose a public health risk. Developing simple and affordable sensors for such pollutants can allow for large-scale monitoring economically. Here, we develop a simple electrochemical sensor for sulfanilamide (SFD) quantification using a phenolic resin substrate and a CO2 laser to pyrolyze the sensor geometry over the substrate. The sensors are modified with carbon nanotubes via a simple drop-casting procedure. The carbon nanotube loading effect the electrochemical performance toward a redox probe and analytical performance for SFD detection is investigated, showing no net benefit beyond 1 mg L-1 of carbon nanotubes. The effects of the modification on the SFD oxidation are shown to be more than just an electrode area effect and possibly attributed to the fast electron transfer kinetics of the carbon nanotubes. SFD detection is performed at small solution volumes under static (800 µL) and hydrodynamic conditions (3 mL) in a fully integrated, miniaturized batch-injection analyses cell. Both methods have a similar linear range from 10.0 to 115.0 µmol L-1 and high selectivity for SFD determination. Both systems are used to quantify SFD in real samples as a proof of concept, showcasing the proposed device's applicability as a sensor for environmental and public health monitoring of SFD.

4.
Anal Chem ; 95(40): 15086-15093, 2023 Oct 10.
Artigo em Inglês | MEDLINE | ID: mdl-37768700

RESUMO

Mixing of graphite and carbon black (CB) alongside recycled poly(lactic acid) and castor oil to create an electrically conductive additive manufacturing filament without the use of solvents is reported herein. The additively manufactured electrodes (AMEs) were electrochemically benchmarked against a commercial conductive filament and a bespoke filament utilizing only CB. The graphite/CB produced a heterogeneous rate constant, k0, of 1.26 (±0.23) × 10-3 cm s-1 and resistance of only 155 ± 15 Ω, compared to 0.30 (±0.03) × 10-3 cm s-1 and 768 ± 96 Ω for the commercial AME. Including graphite within the filament reduced the cost of printing each AME from £0.09, with the CB-only filament, to £0.05. The additive manufacturing filament was successfully used to create an electroanalytical sensing platform for the detection of oxalate within a linear range of 10-500 µM, achieving a sensitivity of 0.0196 µA/µM, LOD of 5.7 µM and LOQ of 18.8 µM was obtained. Additionally, the cell was tested toward the detection of oxalate within a spiked synthetic urine sample, obtaining recoveries of 104%. This work highlights how, using mixed material composites, excellent electrochemical performance can be obtained at a reduced material cost, while also greatly improving the sustainability of the system.

5.
Chemosphere ; 340: 139796, 2023 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-37586488

RESUMO

Here, lab-made graphite and polylactic acid (Gpt-PLA) biocomposite materials were used to additively manufacture electrodes via the fused deposition modeling (FDM) technique for subsequent determination of the explosive 2,4,6-trinitrotoluene (TNT, considered a persistent organic pollutant). The surface of the 3D-printed material was characterized by SEM and Raman, which revealed high roughness and the presence of defects in the graphite structure, which enhanced the electrochemical response of TNT. The 3D-printed Gpt-PLA electrode coupled to square wave voltammetry (SWV) showed suitable performance for fastly determining the explosive residues (around 7 s). Two reduction processes at around -0.22 V and -0.36 V were selected for TNT detection, with linear ranges between 1.0 and 10.0 µM. Moreover, detection limits of 0.52 and 0.66 µM were achieved for both reduction steps. The proposed method was applied to determine TNT in different environmental water samples (tap water, river water, and seawater) without a dilution step (direct analysis). Recovery values between 98 and 106% confirmed the accuracy of the analyses. Additionally, adequate selectivity was achieved even in the presence of other explosives commonly used by military agencies, metallic ions commonly found in water, and also some electroactive camouflage species. Such results indicate that the proposed device is promising to quantify TNT residues in environmental samples, a viable on-site analysis strategy.


Assuntos
Substâncias Explosivas , Grafite , Trinitrotolueno , Trinitrotolueno/análise , Grafite/química , Substâncias Explosivas/análise , Poliésteres , Eletrodos , Água , Impressão Tridimensional , Técnicas Eletroquímicas/métodos
6.
Anal Bioanal Chem ; 2023 Jul 20.
Artigo em Inglês | MEDLINE | ID: mdl-37470814

RESUMO

3D printers utilize cutting-edge technologies to create three-dimensional objects and are attractive tools for engineering compact microfluidic platforms with complex architectures for chemical and biochemical analyses. 3D printing's popularity is associated with the freedom of creating intricate designs using inexpensive instrumentation, and these tools can produce miniaturized platforms in minutes, facilitating fabrication scaleup. This work discusses key challenges in producing three-dimensional microfluidic structures using currently available 3D printers, addressing considerations about printer capabilities and software limitations encountered in the design and processing of new architectures. This article further communicates the benefits of using three-dimensional structures, including the ability to scalably produce miniaturized analytical systems and the possibility of combining them with multiple processes, such as mixing, pumping, pre-concentration, and detection. Besides increasing analytical applicability, such three-dimensional architectures are important in the eventual design of commercial devices since they can decrease user interferences and reduce the volume of reagents or samples required, making assays more reliable and rapid. Moreover, this manuscript provides insights into research directions involving 3D-printed microfluidic devices. Finally, this work offers an outlook for future developments to provide and take advantage of 3D microfluidic functionality in 3D printing. Graphical abstract Creating three-dimensional microfluidic structures using 3D printing will enable key advances and novel applications in (bio)chemical analysis.

7.
Anal Chem ; 95(28): 10634-10643, 2023 Jul 18.
Artigo em Inglês | MEDLINE | ID: mdl-37347237

RESUMO

A simple fabrication method to make electrochemical sensors is reported. The electrodes were fabricated with a commercial filament based on polylactic acid and carbon black (PLA/CB). They were engineered with a three-dimensional (3D) printing pen and poly(methyl methacrylate) template. The optimization parameters included the thickness and diameters of the electrodes. The electrode diameter was restricted by the 3D printing pen's nozzle dimension, and larger diameters generated small cracks on the electrode surface, compromising their analytical signal. The electrode thickness can increase the electrical resistance, affecting their electrochemical response. The fabrication showed reproducibility (RSD = 4%). The electrode surface was easily renewed by sanding the electrodes, making them reusable. Additionally, the proposed sensor provided comparable electrochemical responses over traditional glassy carbon electrodes. Moreover, no (electro)chemical surface treatment was required for sensing applications due to the compromise between the thickness and diameters of the electrodes, effectively translating the filaments' electrical properties to resulting materials. The electrodes' analytical performance was shown for organic and inorganic species, including paraquat, Pb2+, and caffeic acid. As proof of concept, the analytical applicability was demonstrated for total polyphenolic quantification in tea samples. Therefore, this work provides an alternative to fabricating miniaturized electrodes, bringing valuable insights into PLA/CB 3D-printed sensors and opening possibilities for designing electrode arrays. Moreover, the proposed electrodes are promising platforms for paper-based microfluidic systems.

8.
Mikrochim Acta ; 190(7): 276, 2023 06 27.
Artigo em Inglês | MEDLINE | ID: mdl-37368054

RESUMO

Paper-based electrochemical analytical devices (ePADs) have gained significant interest as promising analytical units in recent years because they can be fabricated in simple ways, are low-cost, portable, and disposable platforms that can be applied in various fields. In this sense, paper-based electrochemical biosensors are attractive analytical devices since they can promote diagnose several diseases and potentially allow decentralized analysis. Electrochemical biosensors are versatile, as the measured signal can be improved by using mainly molecular technologies and nanomaterials to attach biomolecules, resulting in an increase in their sensitivity and selectivity. Additionally, they can be implemented in microfluidic devices that drive and control the flow without external pumping and store reagents, and improve the mass transport of analytes, increasing sensor sensitivity. In this review, we focus on the recent developments in electrochemical paper-based devices for viruses' detection, including COVID-19, Dengue, Zika, Hepatitis, Ebola, AIDS, and Influenza, among others, which have caused impacts on people's health, especially in places with scarce resources. Also, we discuss the advantages and disadvantages of the main electrode's fabrication methods, device designs, and biomolecule immobilization strategies. Finally, the perspectives and challenges that need to be overcome to further advance paper-based electrochemical biosensors' applications are critically presented.


Assuntos
Técnicas Biossensoriais , COVID-19 , Nanoestruturas , Infecção por Zika virus , Zika virus , Humanos , COVID-19/diagnóstico , Nanoestruturas/química , Técnicas Biossensoriais/métodos , Dispositivos Lab-On-A-Chip , Teste para COVID-19
9.
Mikrochim Acta ; 190(5): 179, 2023 Apr 12.
Artigo em Inglês | MEDLINE | ID: mdl-37041400

RESUMO

Paper-based analytical devices (PADs) are powerful platforms for point-of-need testing since they are inexpensive devices fabricated in different shapes and miniaturized sizes, ensuring better portability. Additionally, the readout and detection systems can be accomplished with portable devices, allying with the features of both systems. These devices have been introduced as promising analytical platforms to meet critical demands involving rapid, reliable, and simple testing. They have been applied to monitor species related to environmental, health, and food issues. Herein, an outline of chronological events involving PADs is first reported. This work also introduces insights into fundamental parameters to engineer new analytical platforms, including the paper type and device operation. The discussions involve the main analytical techniques used as detection systems, such as colorimetry, fluorescence, and electrochemistry. It also showed recent advances involving PADs, especially combining optical and electrochemical detection into a single device. Dual/combined detection systems can overcome individual barriers of the analytical techniques, making possible simultaneous determinations, or enhancing the devices' sensitivity and/or selectivity. In addition, this review reports on distance-based detection, which is also considered a trend in analytical chemistry. Distance-based detection offers instrument-free analyses and avoids user interpretation errors, which are outstanding features for analyses at the point of need, especially for resource-limited regions. Finally, this review provides a critical overview of the practical specifications of the recent analytical platforms involving PADs, demonstrating their challenges. Therefore, this work can be a highly useful reference for new research and innovation.

10.
Talanta ; 259: 124536, 2023 Jul 01.
Artigo em Inglês | MEDLINE | ID: mdl-37062090

RESUMO

Antibiotics such as tetracycline (TC) are widely prescribed to treat humans or dairy animals. Therefore, it is important to establish affordable devices in laboratories with minimal infrastructure. 3D printing has proven to be a powerful and cost-effective tool that revolutionizes many applications in electrochemical sensing. In this work, we employ a conductive filament based on graphite (Gr) and polylactic acid (PLA) (40:60; w/w; synthesized in our lab) to manufacture 3D-printed electrodes. This electrode was used "as printed" and coupled to batch injection analysis with amperometric detection (BIA-AD) for TC sensing. Preliminary studies by cyclic voltammetry and differential pulse voltammetry revealed a mass transport governed by adsorption of the species and consequent fouling of the redox products on the 3D printed surface. Thus, a simple strategy (solution stirring and application of successive potentials, +0.95 V followed by +1.2 V) was associated with the BIA-AD system to solve this effect. The proposed electrode showed analytical performance comparable to costly conventional electrodes with linear response ranging from 0.5 to 50 µmol L-1 and a detection limit of 0.19 µmol L-1. Additionally, the developed method was applied to pharmaceutical, tap water, and milk samples, which required minimal sample preparation (simple dilution). Recovery values of 92-117% were obtained for tap water and milk samples, while the content found of TC in the capsule was close to the value reported by the manufacturer. These results indicate the feasibility of the method for routine analysis involving environmental, pharmaceutical, and food samples.


Assuntos
Laboratórios , Tetraciclina , Animais , Humanos , Antibacterianos , Impressão Tridimensional , Eletrodos , Água , Preparações Farmacêuticas , Técnicas Eletroquímicas
11.
Mikrochim Acta ; 190(2): 63, 2023 01 21.
Artigo em Inglês | MEDLINE | ID: mdl-36670263

RESUMO

The combination of CO2 laser ablation and electrochemical surface treatments is demonstrated to improve the electrochemical performance of carbon black/polylactic acid (CB/PLA) 3D-printed electrodes through the growth of flower-like Na2O nanostructures on their surface. Scanning electron microscopy images revealed that the combination of treatments ablated the electrode's polymeric layer, exposing a porous surface where Na2O flower-like nanostructures were formed. The electrochemical performance of the fabricated electrodes was measured by the reversibility of the ferri/ferrocyanide redox couple presenting a significantly improved performance compared with electrodes treated by only one of the steps. Electrodes treated by the combined method also showed a better electrochemical response for tyrosine oxidation. These electrodes were used as a non-enzymatic tyrosine sensor for quantification in human urine samples. Two fortified urine samples were analyzed, and the recovery values were 106 and 109%. The LOD and LOQ for tyrosine determination were 0.25 and 0.83 µmol L-1, respectively, demonstrating that the proposed devices are suitable sensors for analyses of biological samples, even at low analyte concentrations.


Assuntos
Terapia a Laser , Nanoestruturas , Humanos , Dióxido de Carbono , Nanoestruturas/química , Oxirredução , Impressão Tridimensional
12.
Talanta ; 240: 123201, 2022 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-34998146

RESUMO

Under controlled dispersion conditions, sample injection towards a detector opened essential fields for the Analytical Chemistry fast development methods. Flow injection analysis (FIA) and batch injection analysis (BIA) systems are crucial for injecting the sample in these analytical methods. The BIA system eliminated the flow manifold, with samples injected directly onto the detector inside the batch injection cell. Paper was slightly evaluated coupled to FIA, and no reports were found associated with BIA. Still, it can potentially reduce the BIA manifold by removing the batch injection cell based on the capillarity properties to disperse the injected solution over the detection system. Hence, this article reported the first work coupling batch-injection analysis and microfluidic paper-based analytical device (BIA-µPAD) with pencil-drawn electrodes directly attached to the paper using a CO2 laser pre-treated chromatographic paper. The laser pretreatment of the paper (optimized conditions: 6.5% laser power, 12 mm s-1 scan rate, and 12 mm output distance) was essential to enhance the electrochemical response for ferri/ferrocyanide redox couple and paracetamol (PAR), as shown by spectroscopic and electrochemical techniques. The proposed BIA-µPAD was evaluated using pharmaceutical paracetamol samples as proof-of-concept (optimized conditions: 15 µL injected volume and 6.4 µL s-1 dispensing rate), obtaining good linearity (R = 0.9961) and recovery values ranging from 95 to 103%. Repeatability (n = 16) and reproducibility (n = 9) tests with 1 mmol L-1 PAR also presented well relative standard deviation (RSD) results of 5.1% and 6.6%, respectively. A sampling frequency of 76 h-1 was obtained, which is a similar value compared with conventional BIA apparatus. Limits of detection and quantification were estimated in 0.046 and 0.154 mmol L-1, respectively. Additionally, an improvement in the current response and the sample throughput was observed when comparing FIA and BIA-µPADs, attesting the applicability of the proposed device and opening for new possibilities related to paper-based devices coupled with flow techniques.


Assuntos
Técnicas Analíticas Microfluídicas , Microfluídica , Técnicas Eletroquímicas , Eletrodos , Dispositivos Lab-On-A-Chip , Papel , Reprodutibilidade dos Testes
13.
Biosensors (Basel) ; 11(12)2021 Nov 30.
Artigo em Inglês | MEDLINE | ID: mdl-34940247

RESUMO

Diphtheria is a vaccine-preventable disease, yet immunization can wane over time to non-protective levels. We have developed a low-cost, miniaturized electroanalytical biosensor to quantify anti-diphtheria toxin (DTx) immunoglobulin G (anti-DTx IgG) antibody to minimize the risk for localized outbreaks. Two epitopes specific to DTx and recognized by antibodies generated post-vaccination were selected to create a bi-epitope peptide, biEP, by synthesizing the epitopes in tandem. The biEP peptide was conjugated to the surface of a pencil-lead electrode (PLE) integrated into a portable electrode holder. Captured anti-DTx IgG was measured by square wave voltammetry from the generation of hydroquinone (HQ) from the resulting immunocomplex. The performance of the biEP reagent presented high selectivity and specificity for DTx. Under the optimized working conditions, a logarithmic calibration curve showed good linearity over the concentration range of 10-5-10-1 IU mL-1 and achieved a limit of detection of 5 × 10-6 IU mL-1. The final device proved suitable for interrogating the immunity level against DTx in actual serum samples. Results showed good agreement with those obtained from a commercial enzyme-linked immunosorbent assay. In addition, the flexibility for conjugating other capture molecules to PLEs suggests that this technology could be easily adapted to the diagnoses of other pathogens.


Assuntos
Técnicas Biossensoriais , Toxina Diftérica , Ensaio de Imunoadsorção Enzimática , Epitopos/imunologia , Imunoensaio , Imunoglobulina G/química , Imunoglobulina G/imunologia
14.
Mikrochim Acta ; 188(11): 388, 2021 10 19.
Artigo em Inglês | MEDLINE | ID: mdl-34668076

RESUMO

For the first time the development of an electrochemical method for simultaneous quantification of Zn2+ and uric acid (UA) in sweat is described using an electrochemically treated 3D-printed working electrode. Sweat analysis can provide important information about metabolites that are valuable indicators of biological processes. Improved performance of the 3D-printed electrode was achieved after electrochemical treatment of its surface in an alkaline medium. This treatment promotes the PLA removal (insulating layer) and exposes carbon black (CB) conductive sites. The pH and the square-wave anodic stripping voltammetry technique were carefully adjusted to optimize the method. The peaks for Zn2+ and UA were well-defined at around - 1.1 V and + 0.45 V (vs. CB/PLA pseudo-reference), respectively, using the treated surface under optimized conditions. The calibration curve showed a linear range of 1 to 70 µg L-1 and 1 to 70 µmol L-1 for Zn2+ and UA, respectively. Relative standard deviation values were estimated as 4.8% (n = 10, 30 µg L-1) and 6.1% (n = 10, 30 µmol L-1) for Zn2+ and UA, respectively. The detection limits for Zn2+ and UA were 0.10 µg L-1 and 0.28 µmol L-1, respectively. Both species were determined simultaneously in real sweat samples, and the achieved recovery percentages were between 95 and 106% for Zn2+ and 82 and 108% for UA.


Assuntos
Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Suor/química , Ácido Úrico/química , Zinco/química
15.
ACS Omega ; 6(1): 594-605, 2021 Jan 12.
Artigo em Inglês | MEDLINE | ID: mdl-33458511

RESUMO

Cocaine (COC) is one of the most widely consumed illegal drugs around the world. Street COC is commonly adulterated with pharmaceutical compounds that mimic or intensify the COC's sensory effect. Adulteration is performed to increase the profit of criminal organizations and each one has their own way of doing it. Therefore, determining the composition of seized COC samples (chemical profile) provides evidence for the police to track criminal organization networks and their activity patterns. Using filter paper as a substrate, we developed a multiple detection paper-based analytical device (PAD) that combines colorimetric and electrochemical measurements to discriminate COC samples according to adulterant's content. A regular graphite lead modified with a gold film made from Au leaf (graphite/Au) to improve electron transfer was used as a working electrode. Silver and Ag/AgCl were used as auxiliary and reference electrodes, respectively. The colorimetric device was patterned using a laser cutter and coupled to the electrochemical device using a double-sided tape, allowing simultaneous analysis to gather more analytical information about COC samples. Graphite/Au was characterized by scanning and transmission electron microscopies and electrochemical assays. The simultaneous colorimetric and electrochemical analyses combined to principal component analysis improved the analytical characterization of COC trial samples and provided a fast discrimination based on the assembled database.

16.
Analyst ; 146(5): 1747-1759, 2021 Mar 07.
Artigo em Inglês | MEDLINE | ID: mdl-33470260

RESUMO

The analysis of 'cutting' or additive agents in cocaine, like benzocaine (BZC), allows police analysts to identify each component of the sample, thus obtaining information like the drugs' provenience. This kind of drug profiling is of great value in tackling drug trafficking. Electropolymerized molecularly imprinted polymers (e-MIPs) on portable screen-printed carbon electrodes (SPCEs) were developed in this study for BZC determination. The MIPs' electropolymerization was performed on a carbon surface using the anaesthetic BZC as the template molecule and 3-amino-4-hydroxybenzoic acid (3,4-AHBA) as the functional monomer. The build-up of this biomimetic sensor was carefully characterized by cyclic voltammetry (CV) and optimized. Cyclic voltammetric investigation demonstrated that BZC oxidation had a complex and pH-dependent mechanism, but at pH 7.4 a single, well-defined oxidation feature was observed. The BZC-MIP interactions were studied by computer-aided theoretical modeling by means of density functional theory (DFT) calculations. The electroanalytical methodology was effectively applied to artificial urine samples; BZC molecular recognition was achieved with a low limit of detection (LOD) of 2.9 nmol L-1 employing square-wave voltammetry (SWV). The e-MIPs were then used to 'fingerprint' genuine cocaine samples, assisted by principal component analysis (PCA), at the central forensic laboratory of the Brazilian Federal Police (BFP) with a portable potentiostat. This electroanalysis provided proof-of-concept that the drugs could be voltammetrically 'fingerprinted' using e-MIPs supported by chemometric analysis.


Assuntos
Cocaína , Impressão Molecular , Benzocaína , Técnicas Eletroquímicas , Eletrodos , Polímeros Molecularmente Impressos , Polímeros
17.
RSC Adv ; 11(3): 1644-1653, 2021 Jan 04.
Artigo em Inglês | MEDLINE | ID: mdl-35424136

RESUMO

Electrochemical Paper-based Analytical Devices (ePADs) are an alternative to traditional portable analytical techniques due to features such as low-cost, easy surface modification with different materials, and high sensitivity. A fast and simple method to fabricate enhanced ePADs using pencil-drawing which involves the CO2 laser treatment of the carbon surface deposited on paper is described. The electrochemical performances of the devices were evaluated using cyclic voltammetry (CV) with different redox probes and electrochemical impedance spectroscopy (EIS). The electrochemical results show that a treated surface presents a lower resistance to charge transfer and changes the approach of the probe and the overlap of its orbitals with the electrode. To investigate the effects of the laser treatment process, chemical and structural characteristics were evaluated using scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS), and Raman spectroscopy. These results indicated that laser treatment promoted the restoration of carbon-carbon double bonds and removed a thin layer of nanodebris present in commercial pencils, resulting in an improvement of the electrochemical kinetics. As a proof-of-concept, the Pencil-Drawing Electrode (PDE) was used for the detection and quantification of furosemide (FUR) in a sample of synthetic urine, exhibiting a limit of detection (LOD) of 2.4 × 10-7 mol L-1. The percentages of recovery of the FUR added to the samples A and B were 95% and 110%, respectively. The analysis using CO2 laser-treated PDE resulted in a fast, simple, and reliable method for this doping agent.

18.
Molecules ; 25(24)2020 Dec 17.
Artigo em Inglês | MEDLINE | ID: mdl-33348539

RESUMO

We studied the dissolution of microcrystalline cellulose (MCC) in binary mixtures of dimethyl sulfoxide (DMSO) and the ionic liquids: allylbenzyldimethylammonium acetate; 1-(2-methoxyethyl)-3-methylimidazolium acetate; 1,8-diazabicyclo [5.4.0]undec-7-ene-8-ium acetate; tetramethylguanidinium acetate. Using chemometrics, we determined the dependence of the mass fraction (in %) of dissolved cellulose (MCC-m%) on the temperature, T = 40, 60, and 80 °C, and the mole fraction of DMSO, χDMSO = 0.4, 0.6, and 0.8. We derived equations that quantified the dependence of MCC-m% on T and χDMSO. Cellulose dissolution increased as a function of increasing both variables; the contribution of χDMSO was larger than that of T in some cases. Solvent empirical polarity was qualitatively employed to rationalize the cellulose dissolution efficiency of the solvent. Using the solvatochromic probe 2,6-dichloro-4-(2,4,6-triphenylpyridinium-1-yl)phenolate (WB), we calculated the empirical polarity ET(WB) of cellobiose (a model for MCC) in ionic liquid (IL)-DMSO mixtures. The ET(WB) correlated perfectly with T (fixed χDMSO) and with χDMSO (fixed T). These results show that there is ground for using medium empirical polarity to assess cellulose dissolution efficiency. We calculated values of MCC-m% under conditions other than those employed to generate the statistical model and determined the corresponding MCC-m% experimentally. The excellent agreement between both values shows the robustness of the statistical model and the usefulness of our approach to predict cellulose dissolution, thus saving time, labor, and material.


Assuntos
Celulose/química , Dimetil Sulfóxido/química , Líquidos Iônicos/química , Solubilidade , Solventes/química , Eletrólitos/química , Imidazóis/química , Compostos de Amônio Quaternário/química , Temperatura
19.
Soft Matter ; 16(33): 7659-7666, 2020 Aug 26.
Artigo em Inglês | MEDLINE | ID: mdl-32724987

RESUMO

While thermal treatment of paper can lead to the formation of aromatic structures via hydrothermal treatment (low temperature) or pyrolysis (high temperature), neither of these approaches allow patterning the substrates. Somewhere in between these two extremes, a handful of research groups have used CO2 lasers to pattern paper and induce carbonization. However, none of the previously reported papers have focused on the possibility to form fluorescent derivatives via laser-thermal engraving. Exploring this possibility, this article describes the possibility of using a CO2 laser engraver to selectively treat paper, resulting in the formation of fluorescent compounds, similar to those present on the surface of carbon dots. To determine the most relevant variables controlling this process, 3 MM chromatography paper was treated using a standard 30 W CO2 laser engraver. Under selected experimental conditions, a blue fluorescent pattern was observed when the substrate was irradiated with UV light (365 nm). The effect of various experimental conditions (engraving speed, engraving power, and number of engraving steps) was investigated to maximize the fluorescence intensity. Through a comprehensive characterization effort, it was determined that 5-(hydroxymethyl)furfural and a handful of related compounds were formed (varying in amount) under all selected experimental conditions. To illustrate the potential advantages of this strategy, that could complement those applications traditionally developed from carbon dots (sensors, currency marking, etc.), a redox-based optical sensor for sodium hypochlorite was developed.

20.
Talanta ; 207: 120270, 2020 Jan 15.
Artigo em Inglês | MEDLINE | ID: mdl-31594601

RESUMO

Since the disclosure of the fibrinogen degradation mechanism, around half a century ago, a significant number of papers have been published related to the clinical relevance of D-dimer, a molecule immune to additional enzymatic decomposition by plasmin. Due to the obliquity of regulating blood coagulation in pathological events, the number of diseases and conditions associated with abnormal levels of D-dimer includes deep vein thrombosis, pulmonary embolism, sepsis, myocardial infarction, disseminated intravascular coagulation, among many others. D-dimer not only is an important player in medical diagnosis but also its role as a prognosis biomarker is being revealed. However, the number of analytical alternative methods has not accompanied this trend, even though novel simple point-of-care devices would certainly boost the relevance of D-dimer in emergency medicine. Some reasons for that could be related to the fact that D-dimer is a challenging analyte present in complex samples like blood. In this manuscript, subsequent to a fibrinogen degradation process introduction, it is provided a historical overview of the early D-dimer assays, followed by an extended focus on innovative solutions, with a spotlight on the electrochemical bioanalytical devices. The discussion is accompanied with a critical analysis and concluding thoughts concerning future perspectives.


Assuntos
Técnicas Biossensoriais/métodos , Produtos de Degradação da Fibrina e do Fibrinogênio/análise , Laboratórios Hospitalares , Pesquisa Translacional Biomédica/métodos , Humanos
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