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1.
Mikrochim Acta ; 191(5): 270, 2024 04 17.
Artigo em Inglês | MEDLINE | ID: mdl-38630200

RESUMO

A comparative analysis of molecularly imprinted polymers based on different synthesis techniques was performed for the recognition of molnupiravir (MOL). The polymerizations were performed with 3-thienyl boronic acid (3-TBA) as a functional monomer by electropolymerization (EP) and with guanine methacrylate (GuaM) as a functional monomer by photopolymerization (PP). Morphological and electrochemical characterizations of the developed sensors were investigated to verify the constructed sensors. Moreover, quantum chemical calculations were used to evaluate changes on the electrode surface at the molecular and electronic levels. The dynamic linear range of both designed sensors under optimized experimental conditions was found to be 7.5 × 10-12-2.5 × 10-10 M and 7.5 × 10-13-2.5 × 10-11 M for EP and PP, respectively. The effect of various interfering agents on MOL peak current was assessed for the selectivity of the study. In the presence of 100 times more interfering agents, the RSD and recovery values were determined. The RSD values of GuaM/MOL@MIP/GCE and poly(Py-co-3-PBA)/MOL@MIP/GCE sensors were found to be 1.99% and 1.72%, respectively. Furthermore, the recovery values of the MIP-based sensors were 98.18-102.69% and 98.05-103.72%, respectively. In addition, the relative selectivity coefficient (k') of the proposed sensor was evaluated, and it exhibited good selectivity for MOL with respect to the NIP sensor. The prepared sensor was successfully applied to determine MOL in commercial serum samples and capsule form. In conclusion, the developed sensors provided excellent reproducibility, repeatability, high sensitivity, and selectivity against the MOL molecule.


Assuntos
Ácidos Borônicos , Citidina/análogos & derivados , Hidroxilaminas , Polímeros Molecularmente Impressos , Reprodutibilidade dos Testes , Eletrodos , Guanina , Metacrilatos
2.
Mikrochim Acta ; 190(10): 397, 2023 09 16.
Artigo em Inglês | MEDLINE | ID: mdl-37715798

RESUMO

Regorafenib (REG) is a diphenylurea derivative oral multikinase inhibitor. It plays an important role in the treatment of colorectal cancer, metastatic gastrointestinal stromal tumors, and hepatocellular carcinoma. Molecularly imprinted polymer (MIP) based glassy carbon electrodes (GCE) were fabricated using photopolymerization (PP) and thermal polymerization (TP) methods. The characterizations of the proposed sensors were investigated by electrochemical techniques, Fourier transform infrared spectroscopy (FT-IR), and scanning electron microscopy (SEM). Several parameters were studied in detail for the optimum conditions of MIP-based sensors, such as dropping volume, photopolymerization and thermal polymerization durations, removal medium and time, and rebinding time. Both sensors' analytical validation and electroanalytical performance comparison were made in different REG concentrations ranging between 0.1 nM and 2.5 nM in standard solution and commercial human serum samples. The limit of detection (LOD) of PP-REG@MIP/GCE and TP-REG@MIP/GCE were 9.13 × 10-12 M and 1.44 × 10-11 M in standard solutions and 2.04 × 10-11 M and 2.02 × 10-11 M in serum samples, respectively. The applicability of the proposed sensors was tested using commercial human serum samples and pharmaceutical form of REG with high recovery values (PP-REG@MIP/GCE and TP REG@MIP/GCE sensors, 99.56-101.59%, respectively). The selectivity of the sensor for REG was investigated in the presence of similar molecules: Sorafenib, Sunitinib, Nilotinib, and Imatinib. The developed techniques and sensors checked the possible biological compounds and ions' effects and storage stability.


Assuntos
Antineoplásicos , Neoplasias Hepáticas , Humanos , Polímeros Molecularmente Impressos , Polimerização , Espectroscopia de Infravermelho com Transformada de Fourier , Carbono
3.
Anal Bioanal Chem ; 414(8): 2775-2785, 2022 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-35112148

RESUMO

In this study, a porous molecularly imprinted electrochemical sensor was successfully fabricated for the selective assay of bisphenol S (BPS) by introducing N-methacryloyl-L tyrosine functional monomer. The molecularly imprinted polymer (MIP)-based sensor (MA-Tyr@MIP/GCE) was prepared via photopolymerization on the glassy carbon electrode and subsequently characterized by using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), scanning electron microscopy (SEM), and Fourier-transform infrared spectroscopy (FTIR). The analytical performance of the sensor was evaluated via CV and differential pulse voltammetry (DPV) measurements. Under the optimized conditions, the rebinding experiment demonstrated that the peak current of the porous MIP-based sensor obviously decreased with the increase of BPS concentration in the concentration range of 1-10 fM. Therefore, the detection limit was determined as 0.171 fM. It should be underlined that MA-Tyr@MIP/GCE exhibited high sensitivity and excellent selectivity because MA-TyrMA-Tyr@MIP/GCE sensor has a higher imprinting factor (IF) toward BPS in respect to competitive analogs, i.e., bisphenol A, bisphenol B, and bisphenol F. The practical application of the sensor also showed good reproducibility and stability for the detection of BPS in human serum and water samples. These results showed MA-Tyr@MIP/GCE successfully applied for the selective recognition of BPS in biological and water samples with high sensitivity and excellent selectivity.


Assuntos
Água Potável , Impressão Molecular , Técnicas Eletroquímicas/métodos , Eletrodos , Humanos , Limite de Detecção , Fenóis , Porosidade , Reprodutibilidade dos Testes , Sulfonas
4.
Anal Bioanal Chem ; 414(19): 5793-5803, 2022 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-35641645

RESUMO

A new electrochemical sensor based on molecularly imprinted tetraethyl orthosilicate (TEOS)-based porous interface was developed for selective recognition of bisphenol F (BPF) in this study. The sensor was prepared by depositing the solution containing TEOS and L-tryptophan (L-Trp) in the presence of cetyltrimethylammonium bromide (CTAB) as a pore-maker via hydrolysis/condensation reaction on the glassy carbon electrode (GCE). While the surface morphology and structure characterization were carried out using Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM), electrochemical characterization was performed through electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The resulted MIP(TEOS:L-Trp)@GCE achieved a wide linear range of 1 × 10-15-1 × 10-14 M for BPF detection with an excellent detection limit of 0.291 fM. Furthermore, the recovery of BPF from spiked bottled water and serum samples varied between 98.83 and 101.03%. These results demonstrate that MIP(TEOS:L-Trp)@GCE was found to be a simple, sensitive, and selective smart interface to detect trace pollution even from complicated samples.


Assuntos
Impressão Molecular , Compostos Benzidrílicos , Carbono/química , Técnicas Eletroquímicas/métodos , Eletrodos , Limite de Detecção , Impressão Molecular/métodos , Polímeros Molecularmente Impressos , Fenóis , Polímeros/química , Dióxido de Silício , Triptofano
5.
Anal Bioanal Chem ; 414(28): 8023-8033, 2022 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-36138122

RESUMO

Tiotropium bromide (TIO) is a long-acting bronchodilator used in the treatment of chronic obstructive pulmonary disease (COPD) and asthma. Specifically, it is used to prevent patients from worsening breathing difficulties. In this study, a new TIO-imprinted electrochemical sensor was designed to detect TIO in serum and pharmaceutical samples. Methacryloyl-L-histidine-cobalt(II) [MAH-Co(II)] has been used as a metal-chelating monomer for synthesizing selective molecularly imprinted polymer (MIP). MIP film has been developed on glassy carbon electrodes using MAH-Co(II) as the functional monomer, 2-hydroxyethyl methacrylate (HEMA) as the basic monomer, and ethylene glycol dimethacrylate (EGDMA) as the cross-linker in the photopolymerization method. The surface characterization of the developed MAH-Co(II)@MIP/GCE electrochemical sensor was done using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Also, the electrochemical behavior of the sensor was provided by differential pulse voltammetry (DPV), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) techniques. Under optimized experimental conditions, the linearity range was in the range of 10-100 fM, and the limit of detection (LOD) and limit of quantitation (LOQ) values were calculated as 2.73 fM and 9.75 fM, respectively. The MAH-Co(II)@MIP/GCE sensor was used to precisely determine TIO in capsule and commercial serum samples. The results demonstrated that the MIP could specifically recognize TIO compared to structurally related drugs and could be reliably applied to the direct determination of drugs from real samples.


Assuntos
Impressão Molecular , Humanos , Impressão Molecular/métodos , Técnicas Eletroquímicas/métodos , Brometo de Tiotrópio , Polímeros/química , Eletrodos , Limite de Detecção
6.
Mikrochim Acta ; 189(6): 225, 2022 05 19.
Artigo em Inglês | MEDLINE | ID: mdl-35585299

RESUMO

A simple, selective, and accurate electrochemical chiral sensor based on molecularly imprinted polymer (MIP) has been developed for sensitive and selective detection of esomeprazole (ESOM). For this purpose, the porous MIP sensor was prepared using tetraethyl orthosilicate (TEOS) and cetyltrimethylammonium bromide (CTAB) in the presence of ß-cyclodextrin (ß-CD) as a chiral recognizing element on a glassy carbon electrode (GCE). The changes in the MIP-layer related to removal and rebinding of the target ESOM were performed via differential pulse voltammetry (DPV) and cyclic voltammetry (CV) by using [Fe(CN)6]3-/4- as the redox probe. The structures of the developed sensor surface were characterized by using scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FTIR). Electrochemical impedance spectroscopy (EIS) was also utilized for a complementary electrochemical characterization. The calibration curve was obtained in the range 1.0 × 10-14-2.0 × 10-13 M with a limit of detection (LOD) of 1.9 × 10-15 M. The developed method has improved the accessibility of binding sites by producing the porous material via hydrolysis/condensation reaction of TEOS in presence of CTAB. The selectivity tests of the developed SiO2-ß-CD@MIP/GCE sensor indicated a high specificity towards ESOM compared with structurally related competitor molecules such as R-omeprazole (R-OM), R-lansoprazole, and S-lansoprazole. The developed sensor was successfully used to determine ESOM in tablets and commercial human serum samples with satisfactory recoveries (100.25 to 100.60%) and precision (RSD 0.46 to 0.66%).


Assuntos
Impressão Molecular , Carbono , Cetrimônio , Técnicas Eletroquímicas/métodos , Esomeprazol , Humanos , Dióxido de Silício , Estereoisomerismo
7.
Biochem Biophys Res Commun ; 578: 42-62, 2021 11 12.
Artigo em Inglês | MEDLINE | ID: mdl-34536828

RESUMO

Apoptosis is a type of cell death caused by the occurrence of both pathological and physiological conditions triggered by ligation of death receptors outside the cell or triggered by DNA damage and/or cytoskeleton disruption. Timely monitoring of apoptosis can effectively help early diagnosis of related diseases and continuous assessment of the effectiveness of drugs. Detecting caspases, a protease family closely related to cellular apoptosis, and its identification as markers of apoptosis is a popular procedure. Biosensors are used for early diagnosis and play a very important role in preventing disease progression in various body sections. Recently, there has been a widespread increase in the desire to use materials made of paper (e.g. nitrocellulose membrane) for Point-of-Care (POC) testing systems since paper and paper-like materials are cheap, abundant and degradable. Microfluidic paper-based analytical devices (µPADs) are highly promising as they are cost-effective, easy to use, fast, precise and sustainable over time and under different environmental conditions. In this review, we focused our efforts on compiling the different approaches on identifying apoptosis pathway while giving brief information about apoptosis and biosensors. This review includes recent advantages in biosensing techniques to simply determine what happened in the cell life and which direction it would continue. As a conclusion, we believed that the review may help to researchers to compare/update the knowledge about diagnosis of the apoptosis pathway while reminding the basic definitions about the apoptosis and biosensor technologies.


Assuntos
Técnicas Biossensoriais/métodos , Caspases/metabolismo , Análise Custo-Benefício/economia , Dano ao DNA , Dispositivos Lab-On-A-Chip/normas , Sistemas Automatizados de Assistência Junto ao Leito/normas , Apoptose/fisiologia , Citoesqueleto/metabolismo , Humanos
8.
Sensors (Basel) ; 17(4)2017 Mar 28.
Artigo em Inglês | MEDLINE | ID: mdl-28350333

RESUMO

Producing molecular imprinting-based materials has received increasing attention due to recognition selectivity, stability, cast effectiveness, and ease of production in various forms for a wide range of applications. The molecular imprinting technique has a variety of applications in the areas of the food industry, environmental monitoring, and medicine for diverse purposes like sample pretreatment, sensing, and separation/purification. A versatile usage, stability and recognition capabilities also make them perfect candidates for use in forensic sciences. Forensic science is a demanding area and there is a growing interest in molecularly imprinted polymers (MIPs) in this field. In this review, recent molecular imprinting applications in the related areas of forensic sciences are discussed while considering the literature of last two decades. Not only direct forensic applications but also studies of possible forensic value were taken into account like illicit drugs, banned sport drugs, effective toxins and chemical warfare agents in a review of over 100 articles. The literature was classified according to targets, material shapes, production strategies, detection method, and instrumentation. We aimed to summarize the current applications of MIPs in forensic science and put forth a projection of their potential uses as promising alternatives for benchmark competitors.


Assuntos
Impressão Molecular , Substâncias para a Guerra Química , Ciências Forenses , Humanos , Polímeros
9.
J Sep Sci ; 39(10): 1998-2005, 2016 May.
Artigo em Inglês | MEDLINE | ID: mdl-27004613

RESUMO

The isolation and purification of ribonucleic acid have attracted attention recently for the understanding of the functions in detail because of the necessity for the treatment of genetic diseases. In this study, guanine-incorporated polymeric cryogels were developed to obtain highly purified ribonucleic acid. The satisfactory purification performance was achieved with the guanine-incorporated poly (2-hydroxyethyl methacrylate-guanine methacrylate) cryogels. The most crucial advantages to use guanine as a functional monomer are to obtain a real natural interaction between guanine on the polymeric material and cytosine on the ribonucleic acid. Moreover, using cryogel with a highly porous structure and high swelling ratio provide advantages of getting more water within the structure to get more analyte to interact. The characterization of cryogels has proved the success of the synthesis and the perfect natural interaction to be taken place between the ligand (guanine methacrylate) and the cytosine in the ribonucleic acid molecules. Although the pores within the structure of cryogels are small, they provide efficient and fast adsorption. The chromatographic separation performance was investigated for different conditions (pH, temperature etc.). The desorption ratio and reusability were also analyzed at the end of the five adsorption-desorption cycles with no significant changes.


Assuntos
Criogéis/química , Guanina/química , Metacrilatos/química , Polímeros/química , RNA/isolamento & purificação , RNA/química
10.
Tuberk Toraks ; 64(4): 283-288, 2016 Dec.
Artigo em Inglês | MEDLINE | ID: mdl-28393717

RESUMO

INTRODUCTION: The aim of this study is to assess the effect of obstructive sleep apnea syndrome (OSAS) severity on leptin levels in children. PATIENTS AND METHODS: Children with habitual snoring underwent overnight polysomnography. Fasting venous blood samples were obtained between 8 AM and 9 AM, following the night of the sleep study. Children with an apnea-hypopnea index of ≥ 5/h were included in the moderate-to-severe OSAS group while those with an apnea-hypopnea index of < 5/h formed the mild OSAS/primary snoring group. RESULT: 47 children (51% male and 49% female; mean age 7.8 ± 2.6 years) were recruited. Twenty seven participants were diagnosed with moderate-to-severe OSAS, and twenty children who had AHI < 5 were included in the mild OSAS/primary snoring. The two groups did not differ regarding age, gender and body mass index z score (p> 0.05). Furthermore there were no differences in log serum leptin levels (p= 0.749). Log serum leptin levels correlated with the BMI z score in the whole study group (p= 0.001; r= 0.499) but they were not associated with apnea-hypopnea index, mean and lowest oxygen saturation during sleep. CONCLUSIONS: Serum leptin levels are affected by adiposity but not by OSAS severity among children with habitual snoring.


Assuntos
Biomarcadores/sangue , Leptina/sangue , Obesidade Infantil , Apneia Obstrutiva do Sono/sangue , Adolescente , Índice de Massa Corporal , Criança , Feminino , Humanos , Lactente , Masculino , Polissonografia , Índice de Gravidade de Doença , Apneia Obstrutiva do Sono/complicações , Ronco/etiologia
11.
Anal Chem ; 86(1): 514-20, 2014 Jan 07.
Artigo em Inglês | MEDLINE | ID: mdl-24364626

RESUMO

Although numerous methods have been reported for the analysis of toxic mercury (Hg(2+)) ions in drinking water, development of simple, rapid, inexpensive, and sensitive sensors still remains a great challenge. Here, we report a simple yet very sensitive colorimetric assay for rapid detection of Hg(2+) in water. The colorimetric assay is based on the aggregation of as-prepared citrate-capped gold nanoparticles (AuNPs) in the presence of Hg(2+) ions and the positively charged amino acid, lysine. The detection limit of this inexpensive colorimetric assay is 2.9 nM, which is below the limit value (10 nM) defined by the U.S. Environmental Protection Agency in drinkable water. Also, the colorimetric response of citrate-capped AuNPs in the presence of lysine is very selective to the Hg(2+). In addition, the colorimetric assay is very fast, and all analyses can be completed within a few minutes.


Assuntos
Colorimetria/métodos , Ouro/química , Lisina/química , Mercúrio/análise , Nanopartículas Metálicas/química , Poluentes Químicos da Água/análise , Colorimetria/normas , Limite de Detecção
12.
J Biomater Sci Polym Ed ; 35(3): 295-305, 2024 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-37982375

RESUMO

Intrauterine devices (IUDs) are widely used in preventing fertilization as contracepting devices. In market, they are produced as T-shaped polyethylene (or propylene) and metal (especially copper) composites. Although the metal component is utilized to provide antibacterial efficacy, prolonged implantation and the presence of a wide range of bacteria flora in the intrauterine environment make IUDs susceptible to bacterial contamination, biofilm formation, and unpleasant infection. In the presented study, the propolis, a natural anti-bacterial/-viral product used for different biomedical applications, coating strategy was applied comparatively in three different ways: coating directly on metal components, coating on polymeric material, and using carrying polymer. In addition, antibacterial activity against Gram-positive (Staphylococcus aureus, S. aureus) and Gram-negative (Escherichia coli, E. coli) bacterial strains were investigated by both dynamic bacterial culture (bacterial inhibition activity) and biofilm (biofilm formation resistance) tests. As a result of 48 h of dynamic bacterial culture; it was determined that the antibacterial inhibition efficiency depending on propolis concentration increased up to 99.5% and 98.5% for E. coli and S. aureus, respectively. In addition, the carrying polymer allows IUDs to cover surfaces more homogeneously, as well as improve antibacterial activity. Similarly; it was determined that biofilm formation resistance was improved by 44.33% for E. coli and by 45.99% for S. aureus with both the propolis concentration and the use of carrying polymer. As a result, it has been revealed that propolis will be classified as an alternative, promising, and effective coating agent for improving antibacterial properties and biofilm formation resistance of IUDs.


Assuntos
Dispositivos Intrauterinos , Própole , Feminino , Humanos , Própole/farmacologia , Staphylococcus aureus , Escherichia coli , Antibacterianos/farmacologia , Polímeros/farmacologia , Biofilmes , Testes de Sensibilidade Microbiana
13.
J Pharm Biomed Anal ; 248: 116283, 2024 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-38850885

RESUMO

This study presented a new method to design a MIP-based electrochemical sensor that could improve the selective and sensitive detection of ipratropium bromide (IPR). The polymeric film was designed using 2-hydroxyethyl methacrylate (HEMA) as the basic monomer, 2-hydroxy-2-methylpropiophenone as the initiator, ethylene glycol dimethacrylate (EGDMA) as the crosslinking agent, and N-methacryloyl-L-aspartic acid (MAAsp) as the functional monomer. The presence of MAAsp results in the functional groups in imprinting binding sites, while the presence of poly(vinyl alcohol) (PVA) allows the generation of porous materials not only for sensitive sensing but also for avoiding electron transport limitations. Electrochemical characterizations of the changes at each stage of the MIP preparation process were confirmed using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). In addition, morphological characterizations of the developed sensor were performed using scanning electron microscopy (SEM), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), and contact angle measurements. Theoretical calculations were also performed to explain/confirm the experimental results better. It was found that the results of the calculations using the DFT approach agreed with the experimental data. The MAAsp-IPR@MIP/GCE sensor was developed using the photopolymerization method, and the sensor surface was obtained by exposure to UV lamp radiation at 365 nm. The improved MIP-based electrochemical sensor demonstrated the ability to measure IPR for standard solutions in the linear operating range of 1.0 × 10-12-1.0 × 10-11 M under optimized conditions. For standard solutions, the limit of detection (LOD) and limit of quantification (LOQ) were obtained as 2.78 × 10-13 and 9.27 × 10-13 M, respectively. The IPR recovery values for the inhalation form were calculated as 101.70 % and 100.34 %, and the mean relative standard deviations (RSD) were less than 0.76 % in both cases. In addition, the proposed modified sensor demonstrated remarkable sensitivity and selectivity for rapid assessment of IPR in inhalation forms. The sensor's unique selectivity is demonstrated by its successful performance even in the presence of IPR impurities.


Assuntos
Técnicas Eletroquímicas , Polímeros Molecularmente Impressos , Polímeros Molecularmente Impressos/química , Técnicas Eletroquímicas/métodos , Técnicas Eletroquímicas/instrumentação , Impressão Molecular/métodos , Modelos Moleculares , Limite de Detecção , Metacrilatos/química , Espectroscopia Dielétrica/métodos , Espectroscopia de Infravermelho com Transformada de Fourier/métodos
14.
Anal Methods ; 16(10): 1480-1488, 2024 Mar 07.
Artigo em Inglês | MEDLINE | ID: mdl-38372557

RESUMO

Rutin (RUT), a natural flavonoid with various beneficial pharmacological actions such as cardioprotective, antioxidant, anti-inflammatory, neuroprotective, etc., is found in the content of many plants that are consumed daily. Due to the healthful effects, RUT is also included in the composition of various herbal supplement samples. Therefore, it is highly important to develop a sensor with high selectivity and sensitivity to determine RUT in complex samples. In this study, it was aimed to take advantage of the cheap, easy, and sensitive nature of electrochemistry and, in addition, to improve the selectivity. For this purpose, the functional monomer selected in the fabricated molecularly imprinted polymer (MIP) was N-methacryloyl-L-aspartic acid (MA-Asp) while photopolymerization (PP) was applied as the polymerization route. After completing critical optimization steps, the developed sensor (MA-Asp@RUT/MIP-GCE) was characterized electrochemically and morphologically. As a result of analytical performance evaluation in standard solution, the linear response of the sensor was found in the concentration range between 1 and 10 pM with a detection limit of 0.269 pM. The recovery studies from plant extract and commercial herbal supplement samples emphasized accuracy and applicability. In imprinting factor studies figuring out quite good selectivity, molecules with a structure similar to RUT were selected as competitors to prove the affinity of the sensor against RUT. Consequently, the MA-Asp@RUT/MIP-GCE sensor offers a more sensitive and selective method thanks to its indirect analysis approach and also stands out with the diversity of its real sample application compared to other available studies.


Assuntos
Impressão Molecular , Polímeros Molecularmente Impressos , Extratos Vegetais , Polímeros/química , Rutina , Técnicas Eletroquímicas/métodos , Impressão Molecular/métodos , Suplementos Nutricionais
15.
Bioelectrochemistry ; 158: 108701, 2024 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-38582008

RESUMO

Herein, we proposed a new approach to design a MIP-based electrochemical sensor with carbon nanofiber (CNF), which could improve its conductivities as well as electrode sensitivity and successful detection of dasatinib (DAS). CNFs are capable of forming high porosity with significant interconnected porous networks. The poly(2-hydroxyethyl-methacrylate-N-methacryloyl-L-tyrosine) (PHEMA-MATyr) copolymer was synthesized in the presence of both CNF and DAS by photopolymerization. After optimization of the parameters, the modified MIP-based electrochemical sensor demonstrated the ability to determine the DAS in the linear working range of 1.0 × 10-14-1.0 × 10-13 M for the standard solution and commercial serum samples with a LOD of 1.76 × 10-15 and 2.46 × 10-15, respectively. Good linearity for DAS was observed with correlation coefficients (r) of 0.996 and 0.997 for the standard solution and commercial serum samples, respectively. The recoveries of the DAS ranged from 99.45 % to 99.53 % for the tablet dosage form and commercial serum samples, with average relative standard deviations below 1.96 % in both cases. The proposed modified sensor demonstrated significant sensitivity and selectivity for the rapid determination of DAS in commercial serum samples and tablet form.


Assuntos
Carbono , Dasatinibe , Técnicas Eletroquímicas , Limite de Detecção , Impressão Molecular , Nanofibras , Nanofibras/química , Dasatinibe/sangue , Carbono/química , Impressão Molecular/métodos , Técnicas Eletroquímicas/métodos , Humanos , Eletrodos
16.
Bioelectrochemistry ; 157: 108655, 2024 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-38310811

RESUMO

In this study, an electrochemical chemosensor that utilizes a conductive polymer-based molecularly imprinted polymer (MIP) surface for rapid and reliable determination of CA125 was devised. A novel method has been applied to fabricate CA125 imprinted polypyrrole nanotubes (MI-PPy NT) via vapor deposition polymerization (VDP) as a recognition element for highly selective and sensitive determination of CA125. The chemosensor was prepared by immobilizing MI-PPy NT onto screen-printed gold electrodes (Au-SPE) and the performance of the sensor was evaluated by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) in terms of selectivity, sensitivity, linear dynamic concentration range (LDR) and limit of detection (LOD). The MI-PPy NT@Au-SPE sensor exhibited high sensitivity (68.57 µA per decade) to the CA125 concentration ranging from 0.1 U mL-1 to 100 U mL-1 at an LOD of 0.4 U mL-1 with a correlation coefficient of 0.9922. The developed chemosensors with their novel design combined with a facile fabrication method, prove to be promising as future state-of-the-art biosensors.


Assuntos
Impressão Molecular , Nanotubos , Neoplasias , Humanos , Polímeros/química , Técnicas Eletroquímicas/métodos , Biomarcadores Tumorais , Impressão Molecular/métodos , Pirróis/química , Limite de Detecção , Eletrodos
17.
Talanta ; 273: 125883, 2024 Jun 01.
Artigo em Inglês | MEDLINE | ID: mdl-38521023

RESUMO

Quercetin (QUE) is a powerful antioxidant and one of the common phenolic compounds found in plants, vegetables, and fruits, which has shown many pharmacological activities. The complex nature of the matrix in which QUE is found and its importance and potential uses in diverse applications force the researchers to develop selective and sensitive sensors. In the present work, a novel molecularly imprinted polymer (MIP)-based electrochemical sensor was fabricated for the selective and sensitive determination of the QUE in plant extracts and food supplements. Tryptophan methacrylate (TrpMA) was chosen as the functional monomer, whereas the photopolymerization (PP) method was applied using a glassy carbon electrode (GCE). Electrochemical and morphological characterizations of the developed sensor (TrpMA@QUE/MIP-GCE) were performed using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and scanning electron microscopy (SEM). The linear range of the developed sensor was determined to be in the range of 1.0-25 pM, while the limit of detection (LOD) was calculated to be 0.235 pM. In conclusion, The TrpMA@QUE/MIP-GCE sensor might be classified as a promising platform for selective and sensitive determination of QUE not only in plant extracts but also in commercial food supplements because of its reliability, reproducibility, repeatability, stability, and fast response time.


Assuntos
Fragaria , Impressão Molecular , Rubus , Polímeros/química , Quercetina , Reprodutibilidade dos Testes , Metanol , Técnicas Eletroquímicas/métodos , Carbono/química , Limite de Detecção , Polímeros Molecularmente Impressos , Eletrodos , Extratos Vegetais
18.
Electrophoresis ; 34(13): 1908-14, 2013 Jul.
Artigo em Inglês | MEDLINE | ID: mdl-23592237

RESUMO

A new type of polymethacrylate-based monolithic column with chiral stationary phase was prepared for the enantioseparation of aromatic amino acids, namely D,L-phenylalanine, D,L-tyrosine, and D,L-tryptophan by CEC. The monolithic column was prepared by in situ polymerization of butyl methacrylate (BMA), N-methacryloyl-L-histidine methyl ester (MAH), and ethylene dimethacrylate (EDMA) in the presence of porogens. The porogen mixture included DMF and phosphate buffer. MAH was used as a chiral selector. FTIR spectrum of the polymethacrylate-based monolith showed that MAH was incorporated into the polymeric structure via in situ polymerization. Some experimental parameters including pH, concentration of the mobile phase, and MAH concentration with regard to the chiral CEC separation were investigated. Single enantiomers and enantiomer mixtures of the amino acids were separately injected into the monolithic column. It was observed that L-enantiomers of aromatic amino acids migrated before D-enantiomers. The reversal enantiomer migration order for tryptophan was observed upon changing of pH. Using the chiral monolithic column (100 µm id and 375 µm od), the best chiral separation was performed in 35:65% ACN/phosphate buffer (pH 8.0, 10 mM) with an applied voltage of 12 kV in CEC. SEM images showed that the chiral monolithic column has a continuous polymeric skeleton and large through-pore structure.


Assuntos
Aminoácidos Aromáticos/química , Eletrocromatografia Capilar/instrumentação , Histidina/análogos & derivados , Metacrilatos/química , Acetonitrilas/química , Aminoácidos Aromáticos/isolamento & purificação , Eletrocromatografia Capilar/métodos , Histidina/química , Pressão , Espectroscopia de Infravermelho com Transformada de Fourier , Estereoisomerismo
19.
Analyst ; 138(21): 6422-8, 2013 Nov 07.
Artigo em Inglês | MEDLINE | ID: mdl-24005005

RESUMO

Procalcitonin (PCT) is a promising biomarker for identification of the origin and severity of sepsis, which is a deadly body infection. In this work, we report the preparation of a surface plasmon resonance (SPR) biosensor which utilizes a molecular imprinted polymer surface for rapid and reliable detection of PCT. The molecular imprinted surface was prepared using a microcontact imprinting technique, in which PCT molecules were first immobilized onto a glass support and brought into contact with a solution of 2-hydroxyethyl methacrylate (HEMA) and ethylene glycol dimethacrylate (EGDMA) on a SPR sensor, then the polymerization process was performed. After removal of the PCT molecules, specific molecular recognition sites were obtained, where PCT molecules can selectively rebind, only at the surface of the polymer matrix. PCT detection studies were carried out using PCT solutions in phosphate buffer and simulated blood plasma (SBP) at different concentrations. The SPR biosensor can detect very low concentrations (9.9 ng mL(-1)) of PCT within approximately 1 h, in both phosphate buffer and SBP. High selectivity of the biosensor against PCT was also demonstrated in the presence of several competitive proteins such as human serum albumin, myoglobin and cytochrome c.


Assuntos
Técnicas Biossensoriais/métodos , Calcitonina/análise , Sistemas Computacionais , Precursores de Proteínas/análise , Ressonância de Plasmônio de Superfície/métodos , Peptídeo Relacionado com Gene de Calcitonina , Humanos , Albumina Sérica/análise , Fatores de Tempo
20.
Biomed Chromatogr ; 27(11): 1524-31, 2013 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-23780689

RESUMO

As alternative hydrophobic adsorbent for DNA adsorption, supermacroporous cryogel disks were synthesized via free radical polymerization. In this study, we have prepared two kinds of cryogel disks: (i) poly(2-hydroxyethyl methacrylate-N-methacryloyl-l-tryptophan) [p(HEMA-MATrp)] cryogel containing specific hydrophobic ligand MATrp; and (ii) monosize p(HEMA-MATrp) particles synthesized via suspension polymerization embedded into p(HEMA) cryogel structure to obtain p(HEMA-MATrp)/p(HEMA) composite cryogel disks. These cryogel disks containing hydrophobic functional group were characterized via swelling studies, Fourier transform infrared spectroscopy, elemental analysis, surface area measurements and scanning electron microscopy. DNA adsorption onto both p(HEMA-MATrp) cryogel and p(HEMA-MATrp)/p(HEMA) composite cryogels was investigated. Maximum adsorption of DNA on p(HEMA-MATrp) cryogel was found to be 15 mg/g polymer. Otherwise, p(HEMA-MATrp)/p(HEMA) composite cryogels significantly increased the DNA adsorption capacity to 38 mg/g polymer. Composite cryogels could be used repeatedly without significant loss on adsorption capacity after 10 repetitive adsorption-desorption cycles.


Assuntos
Criogéis/química , DNA/isolamento & purificação , Poli-Hidroxietil Metacrilato/química , Triptofano/análogos & derivados , Adsorção , Interações Hidrofóbicas e Hidrofílicas
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