Your browser doesn't support javascript.
loading
Mostrar: 20 | 50 | 100
Resultados 1 - 20 de 20
Filtrar
Mais filtros










Base de dados
Intervalo de ano de publicação
1.
Talanta ; 270: 125603, 2024 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-38194860

RESUMO

The present work introduces two novel approaches to fabricate simple and cost-effective pH and temperature probes. Sinusoidal voltage methodologies were employed to electrodeposit polyaniline (PANI) at different growth times (10-20 min) on the surface of an affordable Sonogel-Carbon electrode to conform a robust pH sensor. The presence of PANI and its phases were corroborated by electrochemical means. The sensibility, reversibility and selectivity of the produced sensor were very adequate to apply it in physiological samples. In this regard, the proposed sensor was evaluated in artificial blood serum as well as untreated plasma samples obtaining outstanding results in comparison with a gold reference technique (error <2 %). In addition, a new composite sonogel material, intrinsically modified with multiwalled carbon nanotubes, was attached on top of an electrode couple to one-step fabricate a new temperature probe, relating resistance of the probe with the surroundings temperature. In this case, an optical microscopy characterization was performed to study the sturdiness of the layer. Remarkably, suitable results in terms of sensitivity and selectivity were obtained. The probes were assessed in artificial and untreated plasma samples as well, with the corresponding validation step (error <1 %) by using a commercial temperature probe.

2.
Chemosphere ; 350: 141039, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-38147923

RESUMO

Sulfonamides are among the widespread bacterial antibiotics. Despite this, their quick emergence constitutes a serious problem for ecosystems and human health. Therefore, there is an increased interest in developing relevant detection method for antibiotics in different matrices. In this work, a straightforward, green, and cost-effective protocol was proposed for the preparation of a selective molecularly imprinted membrane (MIM) of sulfamethoxazole (SMX), a commonly used antibiotic. Thus, cellulose acetate was used as the functional polymer, while polyethylene glycol served as a pore-former. The developed MIM was successfully characterized through scanning electron microscopy (SEM), atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), and thermogravimetric analysis (TGA). The MIM was used as a sensing platform in conjunction with a smartphone for optical readout, enabling on-site, selective, and highly sensitive detection of SMX. In this way, a satisfactory imprinting factor of around 3.6 and a limit of detection of 2 ng mL-1 were reached after applying response surface methodologies, including Box-Behnken and central composite designs. Besides, MIM demonstrated its applicability for the accurate and selective detection of SMX in river waters, wastewater, and drugs. Additionally, the MIM was shown to be a valuable sorbent in a solid-phase extraction protocol, employing a spin column setup that offered rapid and reproducible results. Furthermore, the developed sensing platform exhibited notable regeneration properties over multiple cycles and long shelf-life in different storage conditions. The newly developed methodology is of crucial importance to overcome the limitations of classical imprinting polymers. Furthermore, the smartphone-based platform was used to surpass the typically expensive and complicated methods of detection.


Assuntos
Antibacterianos , Impressão Molecular , Humanos , Impressão Molecular/métodos , Sulfametoxazol , Espectroscopia de Infravermelho com Transformada de Fourier , Ecossistema , Extração em Fase Sólida/métodos , Polímeros/química , Adsorção
3.
Biosensors (Basel) ; 13(8)2023 Aug 20.
Artigo em Inglês | MEDLINE | ID: mdl-37622916

RESUMO

The separation of enantiomers plays a critical role in pharmaceutical development, ensuring therapeutic efficacy, safety, and patent protection. It enables the production of enantiopure drugs and enhances our understanding of the properties of chiral compounds. In this study, a straightforward and effective chiral detection strategy was developed for distinguishing between tryptophan (TRP) enantiomers. The approach involved the preparation of a magnetic molecularly imprinted chitosan (MMIC) for preparation of the sample, which was combined with a nitrocellulose membrane (a paper-based analytical device, PAD) integrated with D-TRP covalently grafted with polymethacrylic acid (PAD-PMA_D-TRP). Discriminating between the TRP enantiomers was achieved using AuNPs as a colorimetric probe. Indeed, the presence of D-TRP rapidly induced the aggregation of AuNPs due to its strong affinity to PAD-PMA_D-TRP, resulting in a noticeable change in the color of the AuNPs from red to purple. On the other hand, L-TRP did not induce any color changes. The chiral analysis could be easily performed with the naked eye and/or a smartphone. The developed method exhibited a detection limit of 3.3 µM, and it was successfully applied to detect TRP in serum samples, demonstrating good recovery rates. The proposed procedure is characterized by its simplicity, cost-effectiveness, rapidity, and ease of operation.


Assuntos
Quitosana , Nanopartículas Metálicas , Ouro , Smartphone , Triptofano , Fenômenos Magnéticos
4.
Biosensors (Basel) ; 13(7)2023 Jun 25.
Artigo em Inglês | MEDLINE | ID: mdl-37504077

RESUMO

The authors present a novel sensing platform for a disposable electrochemical, non-enzymatic glucose sensor strip at physiological pH. The sensing material is based on dendritic gold nanostructures (AuNs) resembling feather branches, which are electrodeposited onto a laser-scribed 3D graphene electrode (LSGE). The LSGEs were fabricated via a one-step laser scribing process on a commercially available polyimide sheet. This study investigates several parameters that influence the morphology of the deposited Au nanostructures and the catalytic activity toward glucose electro-oxidation. The electrocatalytic activity of the AuNs-LSGE was evaluated using cyclic voltammetry (CV), linear sweep voltammetry (LSV), and amperometry and was compared to commercially available carbon electrodes prepared under the same electrodeposition conditions. The sensor demonstrated good stability and high selectivity of the amperometric response in the presence of interfering agents, such as ascorbic acid, when a Nafion membrane was applied over the electrode surface. The proposed sensing strategy offers a wide linear detection range, from 0.5 to 20 mM, which covers normal and elevated levels of glucose in the blood, with a detection limit of 0.21 mM. The AuNs-LSGE platform exhibits great potential for use as a disposable glucose sensor strip for point-of-care applications, including self-monitoring and food management. Its non-enzymatic features reduce dependence on enzymes, making it suitable for practical and cost-effective biosensing solutions.


Assuntos
Técnicas Biossensoriais , Grafite , Nanoestruturas , Técnicas Eletroquímicas , Eletrodos , Glucose , Ouro/química , Grafite/química , Lasers , Nanoestruturas/química
5.
Foods ; 12(9)2023 Apr 23.
Artigo em Inglês | MEDLINE | ID: mdl-37174286

RESUMO

There is an increasing interest in food science for high-quality natural products with a distinct geographical origin, such as saffron. In this work, the excitation-emission matrix (EEM) and synchronous fluorescence were used for the first time to geographically discriminate between Moroccan saffron from Taroudant, Ouarzazate, and Azilal. Moreover, to differentiate between Afghan, Iranian, and Moroccan saffron, a unique fingerprint was assigned to each sample by visualizing the EEM physiognomy. Moreover, principal component analysis (LDA) and linear discriminant analysis (LDA) were successfully applied to classify the synchronous spectra of samples. High fluorescence intensities were registered for Ouarzazate and Taroudant saffron. Yet, the Azilal saffron was distinguished by its low intensities. Furthermore, Moroccan, Afghan, and Iranian saffron were correctly assigned to their origins using PCA and LDA for different offsets (Δλ) (20-250 nm) such that the difference in the fluorescence composition of the three countries' saffron was registered in the following excitation/emission ranges: 250-325 nm/300-480 nm and 360-425 nm/500-550 nm. These regions are characterized by the high polyphenolic content of Moroccan saffron and the important composition of Afghan saffron, including vitamins and terpenoids. However, weak intensities of these compounds were found in Iranian saffron. Furthermore, a substantial explained variance (97-100% for PC1 and PC2) and an important classification rate (70-90%) were achieved. Thus, the non-destructive applied methodology of discrimination was rapid, straightforward, reliable, and accurate.

6.
Mikrochim Acta ; 190(5): 168, 2023 Apr 04.
Artigo em Inglês | MEDLINE | ID: mdl-37012526

RESUMO

A new electrochemical sensor device has been developed through the modification of a polyaniline-silicon oxide network with carbon black (CB). Enhanced electrical conductivity and antifouling properties have been achieved due to the integration of this cheap nanomaterial into the bulk of the sensor. The structure of the developed material was characterized using Fourier transform infrared spectroscopy, energy-dispersive X-ray spectroscopy, and scanning electron microscopy techniques. Cyclic voltammetry was used to characterize electrochemically the Sonogel-Carbon/Carbon Black-PANI (SNG-C/CB-PANI) sensor device. In addition, differential pulse voltammetry was employed to evaluate the analytical response of the sensor towards sundry chlorophenols, common environmental hazards in aqueous ecosystems. The modified sensor material showed excellent antifouling properties, which led to a better electroanalytical performance than the one displayed with the bare sensor. Notably, a sensitivity of 5.48 × 103 µA mM-1 cm-2 and a limit of detection of 0.83 µM were obtained in the determination of 4-chloro-3-methylphenol (PCMC) at a working potential of 0.78 V (vs. 3 M Ag/AgCl/KCl), along with proficient values of reproducibility and repeatability (relative standard deviation < 3%). Finally, the analysis of PCMC was carried out in multiple validated water samples using the synthesized SNG-C/CB-PANI sensor device, obtaining excellent results of recovery values (97-104%). The synergetic effect of polyaniline and carbon black leads to novel antifouling and electrocatalytic effects that improve the applicability of this sensor in sample analysis versus complex conventional devices.

7.
Sensors (Basel) ; 22(21)2022 Nov 03.
Artigo em Inglês | MEDLINE | ID: mdl-36366146

RESUMO

Reusable Sonogel-Carbon electrodes containing carbon black (SNGC-CB) have been used for the electrochemical analysis of caffeic acid (CA) in real matrices. Measurements were firstly performed in standard solutions, in which SNGC-CB electrodes allowed the electrochemical determination of CA with high sensitivity and low limit of detection, equal to 0.76 µM. The presence of CB nanostructures in the formulation led to improved performances with respect to pristine SNGC electrodes. Then, measurements were performed in four instant coffees of different brands. A comparison between the results obtained by electrochemical, chromatographic and spectroscopic methods showed that SBGC-CB electrodes represent a simple and economic tool for the rapid assessment of caffeic acid-related molecules in instant coffees.


Assuntos
Carbono , Café , Carbono/química , Eletrodos , Ácidos Cafeicos/análise , Ácidos Cafeicos/química , Técnicas Eletroquímicas/métodos , Limite de Detecção
8.
Biosensors (Basel) ; 12(11)2022 Oct 25.
Artigo em Inglês | MEDLINE | ID: mdl-36354428

RESUMO

Monitoring of lactate is spreading from the evident clinical environment, where its role as a biomarker is notorious, to the agrifood ambit as well. In the former, lactate concentration can serve as a useful indicator of several diseases (e.g., tumour development and lactic acidosis) and a relevant value in sports performance for athletes, among others. In the latter, the spotlight is placed on the food control, bringing to the table meaningful information such as decaying product detection and stress monitoring of species. No matter what purpose is involved, electrochemical (bio)sensors stand as a solid and suitable choice. However, for the time being, this statement seems to be true only for discrete measurements. The reality exposes that real and continuous lactate monitoring is still a troublesome goal. In this review, a critical overview of electrochemical lactate (bio)sensors for clinical and agrifood situations is performed. Additionally, the transduction possibilities and different sensor designs approaches are also discussed. The main aim is to reflect the current state of the art and to indicate relevant advances (and bottlenecks) to keep in mind for further development and the final achievement of this highly worthy objective.


Assuntos
Técnicas Biossensoriais , Ácido Láctico , Humanos
9.
Food Chem ; 393: 133417, 2022 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-35691065

RESUMO

A fast, precise and inexpensive alternative for evaluating the antioxidant activity (AA) in walnut kernel extracts is proposed. Traditional ABTS assay and an electrochemical index approach have been applied to evaluate the AA in walnuts. A fast and efficient defatting of the walnuts by ultrasound assisted extraction (UAE) was carried out. Later, for the extraction of polyphenolic compounds, a procedure based on UAE in ethanolic medium was used. The AA of the sample ethanolic extracts was expressed as both % of inhibition by the ABTS spectrophotometric method and the electrochemical index approach (EI) obtained by the ratio between current and potential peak values using differential pulse voltammetry (DPV) at a Sonogel-Carbon electrode. The behaviour of the EI approach have been explored using six polyphenols standards and walnut kernel extracts at pH 2. All the polyphenols appeared at an oxidation potential between 0.476 and 0.778 V. Eleven samples available to consumers were analysed. A high significant correlation (R2 = 0.927) between the spectrophotometric measurements and the EI approach of the walnut extracts was obtained.


Assuntos
Antioxidantes , Juglans , Antioxidantes/química , Flavonoides/química , Juglans/química , Extratos Vegetais/química , Polifenóis/química
10.
Sensors (Basel) ; 21(24)2021 Dec 18.
Artigo em Inglês | MEDLINE | ID: mdl-34960563

RESUMO

In this work, template-free nanostructured conducting polymers (nCPs)-embedded gold nanoparticles (AuNPs) from aniline, thiophene and 3,4-ethylenedioxythiophene have been prepared via a one-pot sonochemical method. The synthesis of the nanocomposite (nCPs-AuNPs) was achieved in a short period of time (5-10 min), by applying high-energy ultrasound to an aqueous mixture of a CP precursor monomer and KAuCl4, in the presence of LiClO4 as dopant. The synthesis process is simpler, greener and faster in comparison to other procedures reported in the literature. Remarkably, bulk quantities of doped polyaniline PANI-AuNPs nanofibers were obtained. Subsequently, they were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDS) and Fourier transform infrared spectroscopy (FTIR), as well as by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). PANI-AuNPs nanofibers were also employed as immobilization matrix for a benchmark enzyme, glucose oxidase (GOX). Finally, glucose was determined in real samples of white and red wines by using the so-obtained GOX-PANI-AuNPs/Sonogel-Carbon biosensor, providing outstanding recoveries (99.54%). This work may offer important insights into the synthesis of nanostructured conducting polymers and also stimulates the exploration of the applications of these nanocomposites, especially in research fields such as (bio)sensors, catalysis and composite materials.


Assuntos
Nanopartículas Metálicas , Nanofibras , Compostos de Anilina , Ouro
11.
Anal Chem ; 93(47): 15744-15751, 2021 11 30.
Artigo em Inglês | MEDLINE | ID: mdl-34783529

RESUMO

We present a pH nanosensor conceived for single intracellular measurements. The sensing architecture consisted of a two-electrode system evaluated in the potentiometric mode. We used solid-contact carbon nanopipette electrodes tailored to produce both the indicator (pH nanosensor) and reference electrodes. The indicator electrode was a membrane-based ion-selective electrode containing a receptor for hydrogen ions that provided a favorable selectivity for intracellular measurements. The analytical features of the pH nanosensor revealed a Nernstian response (slope of -59.5 mV/pH unit) with appropriate repeatability and reproducibility (variation coefficients of <2% for the calibration parameters), a fast response time (<5 s), adequate medium-term drift (0.7 mV h-1), and a linear range of response including physiological and abnormal cell pH levels (6.0-8.5). In addition, the position and configuration of the reference electrode were investigated in cell-based experiments to provide unbiased pH measurements, in which both the indicator and reference electrodes were located inside the same cell, each of them inside two neighboring cells, or the indicator electrode inside the cell and the reference electrode outside of (but nearby) the studied cell. Finally, the pH nanosensor was applied to two cases: (i) the tracing of the pH gradient from extra-to intracellular media over insertion into a single PC12 cell and (ii) the monitoring of variations in intracellular pH in response to exogenous administration of pharmaceuticals. It is anticipated that the developed pH nanosensor, which is a label-free analytical tool, has high potential to aid in the investigation of pathological states that manifest in cell pH misregulation, with no restriction in the type of targeted cells.


Assuntos
Eletrodos Seletivos de Íons , Prótons , Concentração de Íons de Hidrogênio , Potenciometria , Reprodutibilidade dos Testes
12.
Sensors (Basel) ; 21(15)2021 Jul 22.
Artigo em Inglês | MEDLINE | ID: mdl-34372213

RESUMO

Conducting polymers (CPs) are extensively studied due to their high versatility and electrical properties, as well as their high environmental stability. Based on the above, their applications as electronic devices are promoted and constitute an interesting matter of research. This review summarizes their application in common electronic devices and their implementation in electronic tongues and noses systems (E-tongues and E-noses, respectively). The monitoring of diverse factors with these devices by multivariate calibration methods for different applications is also included. Lastly, a critical discussion about the enclosed analytical potential of several conducting polymer-based devices in electronic systems reported in literature will be offered.


Assuntos
Técnicas Biossensoriais , Polímeros , Nariz Eletrônico , Eletrônica , Língua
13.
Mater Sci Eng C Mater Biol Appl ; 123: 112023, 2021 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-33812640

RESUMO

The present study is focused on the ultrafast and green synthesis, via the co-precipitation method, of magnetic nanoparticles (MNPs) based on iron oxides using design of experiments (DOE) and high energy sonochemical approach, considering two main factors: amplitude (energy) of the ultrasound probe and sonication time. The combination of these techniques allowed the development of a novel one-minute green synthesis, which drastically reduced the amount of consumed energy, solvents, reagents, time and produced residues. This green sonochemical synthesis permitted to obtain mean particle sizes of 11 ± 2 nm under the optimized conditions of amplitude = 40% (2826 J) and time = 1 min. Their composition, structure, size, morphology and magnetic properties were assessed through X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), scanning and transmission electron microscopy (SEM & TEM), and vibrating sample magnetometry (VSM). The characterization results indicate the proper formation of MNPs, and the correct functionalization of MNPs with different coating agents. The functionalized MNPs were used as: i) biosensor, which could detect mercury in water in the range of 0.030-0.060 ppm, and ii) support onto which polyclonal antibodies were anchored and successfully bound to an osteosarcoma cell line expressing the target protein (TRIB2-GFP), as part of an immunoprecipitation assay.


Assuntos
Nanopartículas de Magnetita , Imunoprecipitação , Nanopartículas Magnéticas de Óxido de Ferro , Fenômenos Magnéticos , Magnetismo , Espectroscopia de Infravermelho com Transformada de Fourier
14.
ACS Sens ; 6(3): 1129-1137, 2021 03 26.
Artigo em Inglês | MEDLINE | ID: mdl-33566575

RESUMO

We present herein the most complete characterization of microneedle (MN) potentiometric sensors for pH transdermal measurements for the time being. Initial in vitro assessment demonstrated suitable analytical performances (e.g., Nernstian slope, linear range of response from 8.5 to 5.0, and fast response time) in both buffer media and artificial interstitial fluid (ISF). Excellent repeatability and reproducibility together with adequate selectivity and resiliency facilitate the appropriateness of the new pH MN sensor for transdermal ISF analysis in healthcare. The ability to resist skin insertions was evaluated in several ex vivo setups using three different animal skins (i.e., chicken, pork, and rat). The developed pH MN sensor was able to withstand from 5 to 10 repetitive insertions in all the skins considered with a minimal change in the calibration graph (<3% variation in both slope and intercept after the insertions). Ex vivo pH measurements were validated by determining the pH with the MN sensor and a commercial pH electrode in chicken skin portions previously conditioned at several pH values, obtaining excellent results with an accuracy of <1% and a precision of <2% in all cases. Finally, pH MN sensors were applied for the very first time to transdermal measurements in rats together with two innovative validation procedures: (i) measuring subcutaneous pH directly with a commercial pH microelectrode and (ii) collecting ISF using hollow MNs and then the pH measurement of the sample with the pH microelectrode. The pH values obtained with pH MN sensors were statistically more similar to subcutaneous measurements, as inferred by a paired sample t-test at 95% of confidence level. Conveniently, the validation approaches could be translated to other analytes that are transdermally measured with MN sensors.


Assuntos
Técnicas Biossensoriais , Animais , Eletrodos , Concentração de Íons de Hidrogênio , Potenciometria , Ratos , Reprodutibilidade dos Testes
15.
Biomacromolecules ; 22(2): 949-960, 2021 02 08.
Artigo em Inglês | MEDLINE | ID: mdl-33502851

RESUMO

We have developed an innovative methodology to overcome the lack of techniques for real-time assessment of degradable biomedical polymers at physiological conditions. The methodology was established by combining polymer characterization techniques with electrochemical sensors. The in vitro hydrolytic degradation of a series of aliphatic polyesters was evaluated by following the molar mass decrease and the mass loss at different incubation times while tracing pH and l-lactate released into the incubation media with customized miniaturized electrochemical sensors. The combination of different analytical approaches provided new insights into the mechanistic and kinetics aspects of the degradation of these biomedical materials. Although molar mass had to reach threshold values for soluble oligomers to be formed and specimens' resorption to occur, the pH variation and l-lactate concentration were direct evidence of the resorption of the polymers and indicative of the extent of chain scission. Linear models were found for pH and released l-lactate as a function of mass loss for the l-lactide-based copolymers. The methodology should enable the sequential screening of degradable polymers at physiological conditions and has potential to be used for preclinical material's evaluation aiming at reducing animal tests.


Assuntos
Poliésteres , Polímeros , Animais , Materiais Biocompatíveis , Hidrólise , Ácido Láctico
16.
Sensors (Basel) ; 22(1)2021 Dec 24.
Artigo em Inglês | MEDLINE | ID: mdl-35009659

RESUMO

In this work, the development of an electrochemical sensor for melatonin determination is presented. The sensor was based on Sonogel-Carbon electrode material (SNGCE) and Au nanoparticles (AuNPs). The low-cost and environmentally friendly SNGCE material was prepared by the ultrasound-assisted sonogel method. AuNPs were prepared by a chemical route and narrow size distribution was obtained. The electrochemical characterization of the SNGCE/AuNP sensor was carried out by cyclic voltammetry in the presence of a redox probe. The analytical performance of the SNGCE/AuNP sensor in terms of linear response range, repeatability, selectivity, and limit of detection was investigated. The optimized SNGCE/AuNP sensor displayed a low detection limit of 8.4 nM melatonin in synthetic samples assessed by means of the amperometry technique. The potential use of the proposed sensor in real sample analysis and the anti-matrix capability were assessed by a recovery study of melatonin detection in human peripheral blood serum with good accuracy.


Assuntos
Melatonina , Nanopartículas Metálicas , Carbono , Técnicas Eletroquímicas , Eletrodos , Ouro , Humanos , Limite de Detecção
17.
Ultrason Sonochem ; 58: 104670, 2019 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-31450357

RESUMO

In this work, a comparative study of the effect of various solvents on the synthesis of magnetic molecularly imprinted polymers (MMIPs) based on the use of high-power ultrasound probe is reported for the first time. Dimethylsulfoxide (DMSO), dimethylformamide (DMF), ethanol, acetonitrile and acetone were studied as solvents for the synthesis of MMIPs. Several crucial experimental conditions such as the time of synthesis and the applied amplitude were investigated. DMSO, DMF and ethanol were successfully used for ultrasound-assisted synthesis of MMIPs. However, for the polymerization performed using acetonitrile and acetone, no significant conversion to product was observed. Under optimal conditions for each solvent tested, the synthesized MMIPs were characterized using several techniques such as Scanning/Transmission Electron Microscopy (SEM and STEM modes), X-Ray Diffraction, Fourier Transform Infra-Red Spectroscopy, Thermal Gravimetric Analysis and Vibrating Sample Magnetometer system. The study of adsorption time of MMIPs showed that fast adsorption occurred due to the presence of specific imprinted sites on the surface. Moreover, isotherm study showed that the experimental equilibrium data fitted well with Freundlich model. The results of selectivity study indicated that MMIPs could selectively recognize the target molecule. Due to its high adsorption properties and easiness of preparation, MMIP-DMSO was used successfully as adsorbent material in solid-phase extraction coupled to a colorimetric method for sulfamethoxazole (SMX). After optimizing analytical conditions, a calibration plot was performed in the concentration range from 0.2 to 5 µg·mL-1 with limits of detection and quantitation of 0.06 and 0.2 µg·mL-1, respectively. The developed procedure was applied successfully for SMX determination in spiked tap and mineral waters showing satisfactory recoveries. Besides, reusability study demonstrated that MMIP could be reused at least 8 times keeping good binding capacity.

18.
Talanta ; 204: 57-62, 2019 Nov 01.
Artigo em Inglês | MEDLINE | ID: mdl-31357336

RESUMO

In this work, a method for the determination of phosphorus in walnuts has been developed due to the fact that there is no specific method for this purpose. A closed-vessel microwave-assisted digestion of the samples was optimized and a modified molybdenum blue spectrophotometric method was carried out with excellent precision and selectivity. To differentiate assimilable and non-assimilable phosphorus, an easy extraction procedure using 1 M NH4Cl was used. FTIR spectra ensured that the phytate extraction was successful. A sampling of thirteen different walnuts available to consumers from different crops and geographical origin was performed. Comparative statistical tools to differentiate walnuts were also carried out. Significant differences based on total content of phosphorus were obtained. Finally, a correlation study between total phosphorus concentration and the non-assimilable fraction showed a non-linear relationship (R2 = 0.435). Therefore, in relation to consumer health the total phosphorus determination must be complemented with information about assimilable phosphorus.


Assuntos
Juglans/química , Nozes/química , Fósforo/análise , Molibdênio/química , Extração em Fase Sólida/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
19.
Ultrason Sonochem ; 53: 226-236, 2019 May.
Artigo em Inglês | MEDLINE | ID: mdl-30686595

RESUMO

In this paper, we report for the first time a novel, simple and fast method for the synthesis of magnetic molecularly imprinted polymers (Mag-MIPs) based on high-energy ultrasound probe. Sulfamethoxazole (SMX) was used as template molecule, methacrylic acid as functional monomer, ethylene glycole dimethacrylate as crosslinking agent and magnetic nanoparticles (NPs) as the supporting core. The effects of time (5, 7.5 and 10 min) and the applied amplitude (20, 30, 40, 50 and 60%) using the ultrasound probe for the synthesis of Mag-MIPs were studied and optimized. By applying the proposed synthesis method, the US-magMIPs synthesis time was satisfactorily reduced from several hours to a few minutes (7.5 min) in a simple way. For comparison purposes, the Mag-MIP and the non imprinted polymer (MagNIP) were also synthesized employing an ultrasound bath assisted approach (2 h, 65 °C). Magnetic NPs and US-magMIPs synthesized by both ways were investigated by means of several characterization techniques such as Fourier Transform Infrared (FT-IR) spectroscopy, Scanning/Transmission electron microscopy (SEM and STEM modes), X-Ray Diffraction (XRD), Vibrating Sample Magnetometer (VSM) and Dynamic Light Scattering (DLS). The results obtained confirms clearly the formation of magnetic NPs and their successful decoration by the imprinted polymer in both synthesis ways. The sulfonamide binding efficiency of US-magMIPs synthesized by the ultrasound probe and ultrasound bath were investigated according to the adsorption isotherm. The obtained results showed that the US-magMIP synthesized with the probe has more binding capacity compared to the one synthesized with US bath. The adsorption time was studied and both synthesized US-magMIPs reached the maximum adsorption capacity toward SMX after 1 h and the US-magMIP probe tends to have more easiness to bind SMX in less time. The selectivity studies of the synthesized US-magMIPs based on probe and bath showed a high affinity for SMX compared to its structural analogues such as sulfadiazine, sulfamerazine and sulfacetamide.

20.
Sensors (Basel) ; 19(1)2018 Dec 25.
Artigo em Inglês | MEDLINE | ID: mdl-30585182

RESUMO

The application of a novel Poly(3,4-ethylenedioxythiophene)-Tyrosinase/Sonogel-Carbon electrode (PEDOT-Tyr/SNGC) biosensor to beers and wines analysis is proposed. This biosensor implies a new Sinusoidal Current (SC) electrodeposition method to immobilize the enzyme generating a nanostructure surface. The biosensors were characterized electrochemically, employing cyclic voltammetry and electrochemical impedance spectroscopy. Sensitivity, limit of detection, and correlation coefficients of the linear fitting were 2.40 × 10-4 µA·µM-1, 4.33 µM, and R² = 0.9987, respectively. Caffeic acid is used as the reference polyphenol. A sampling of nine beers (four lager, three stout, and two non-alcoholic beers), and four wines (three red and one white wine) purchased in a local store was performed. The Polyphenol indeces for beers and wines have been assessed using the proposed biosensor, and the obtained values are in agreement with the literature data. Antioxidant properties of the samples using the 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid (ABTS) radical spectrophotometric method were also evaluated. The correlation between the polyphenol index and the antioxidant capacity was obtained for beers and wines.

SELEÇÃO DE REFERÊNCIAS
DETALHE DA PESQUISA
...