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1.
Mikrochim Acta ; 191(5): 230, 2024 Apr 02.
Artigo em Inglês | MEDLINE | ID: mdl-38565804

RESUMO

A novel molecularly imprinted electrochemical sensor is presented based on one-dimensional ultrathin manganese oxide nanowires/two-dimensional molybdenum titanium carbide MXene (MnO2NWs@Mo2TiC2 MXene) for fenitrothion (FEN) determination. After the synthesis of MnO2NWs@Mo2TiC2 MXene ionic nanocomposite was successfully completed with a facile hydrothermal and the pillaring methods, a new type molecular imprinted electrochemical sensor based on MnO2NWs@Mo2TiC2 MXene was constructed with cyclic voltammetry (CV) polymerization including pyrrole monomer and FEN target molecule. After the characterization studies including spectroscopic, electrochemical and microscopic methods, the analytical applications of the prepared sensor were performed. A linearity of 1.0×10-9-2.0×10-8 mol L-1 was obtained and the values of the quantification limit (LOQ) and the detection limit (LOD) were 1.0×10-9 mol L-1 and 3.0×10-10 mol L-1, respectively. The studies of selectivity, stability and reproducibility of the constructed sensor based on MnO2NWs@Mo2TiC2 nanocomposite and molecularly imprinting polymer (MIP) were carried out in detail. Finally, the developed sensor was applied to white flour samples with the values close to 100%.

2.
Analyst ; 148(16): 3827-3834, 2023 Aug 07.
Artigo em Inglês | MEDLINE | ID: mdl-37432049

RESUMO

A novel electrochemical detection method based on a nickel ferrite@graphene (NiFe2O4@Gr) nanocomposite-containing molecularly imprinted polymer (MIP) was developed for the sensitive determination of butylated hydroxyanisole (BHA). After successful completion of the nanocomposite production under hydrothermal conditions, the NiFe2O4@Gr nanocomposite and a novel molecularly imprinted sensor based on the NiFe2O4@Gr nanocomposite were characterized using microscopic, spectroscopic and electrochemical techniques. According to the characterization results, the synthesis of the core-shell type NiFe2O4@Gr nanocomposite with high purity and efficiency has been proved to be successful. After successful modification of a cleaned glassy carbon electrode (GCE) with the NiFe2O4@Gr nanocomposite, analytical applications were started with the prepared BHA printed GCE. This novel molecularly imprinted electrochemical sensor for BPA detection demonstrated a linearity of 1.0 × 10-11-1.0 × 10-9 M and a low detection limit (LOD, 3.0 × 10-12 M). In addition, the BHA imprinted polymer based on the NiFe2O4@Gr nanocomposite also exhibited excellent selectivity, stability, reproducibility and reusability performances in flour analysis.

3.
Mikrochim Acta ; 190(7): 262, 2023 06 17.
Artigo em Inglês | MEDLINE | ID: mdl-37329340

RESUMO

Zearalenone (ZEN) is a mycotoxin that has a carcinogenic effect and is often found at a high rate in frequently consumed foods. In this study, a characteristic molecular imprinted quartz crystal microbalance (QCM) sensor based on molybdenum disulfide nanoparticle (MoS2NPs)-multiwalled carbon nanotube (MWCNT) nanocomposite (MoS2NPs-MWCNTs) is presented for selective determination of ZEA in rice samples. Firstly, molybdenum disulfide nanoparticle (MoS2NP)-multiwalled carbon nanotube nanocomposites were characterized by using microscopic, spectroscopic, and electrochemical techniques. Then, ZEA-imprinted QCM chip was prepared in the presence of methacryloylamidoglutamicacid (MAGA) as monomer, N,N'-azobisisobutyronitrile (AIBN) as initiator, and ZEA as target molecule by using UV polymerization. The sensor revealed a linearity toward ZEA in the range 1.0-10.0 ng L-1 with a detection limit (LOD) of 0.30 ng L-1. The high repeatability, reusability, selectivity, and stability of the developed sensor enable reliable ZEA detection in rice samples.


Assuntos
Impressão Molecular , Nanocompostos , Nanotubos de Carbono , Zearalenona , Técnicas de Microbalança de Cristal de Quartzo/métodos , Impressão Molecular/métodos , Limite de Detecção
4.
Mikrochim Acta ; 189(6): 242, 2022 06 02.
Artigo em Inglês | MEDLINE | ID: mdl-35654985

RESUMO

The early diagnosis of major diseases such as cancer is typically a major issue for humanity. Human α-fetoprotein (AFP) as a sialylated glycoprotein is of approximately 68 kD molecular weight and is considered to be a key biomarker, and an increase in its level indicates the presence of liver, testicular, or gastric cancer. In this study, an electrochemical AFP immunosensor based on Fe3O4NPs@covalent organic framework decorated gold nanoparticles (Fe3O4 NPs@COF/AuNPs) for the electrode platform and double-coated magnetic nanoparticles (MNPs) based on SiO2@TiO2 (MNPs@SiO2@TiO2) nanocomposites for the signal amplification was fabricated. The immobilization of anti-AFP capture antibody was successfully performed on Fe3O4 NPs@COF/AuNPs modified electrode surface by amino-gold affinity, while the conjugation of anti-AFP secondary antibody on MNPs@SiO2@TiO2 was achieved by the electrostatic/ionic interactions. Transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) analysis, cyclic voltammetry (CV), square wave voltammetry (SWV), and electrochemical impedance spectroscopy (EIS) techniques were used to characterize the nanostructures in terms of physical and electrochemical features. The limit of detection (LOD) was 3.30 fg mL-1. The findings revealed that the proposed electrochemical AFP immunosensor can be effectively used to diagnose cancer.


Assuntos
Técnicas Biossensoriais , Nanopartículas de Magnetita , Estruturas Metalorgânicas , Técnicas Biossensoriais/métodos , Ouro/química , Humanos , Imunoensaio , Nanopartículas de Magnetita/química , Dióxido de Silício , Titânio , alfa-Fetoproteínas/análise
5.
Anal Bioanal Chem ; 413(9): 2481-2492, 2021 Apr.
Artigo em Inglês | MEDLINE | ID: mdl-33544162

RESUMO

TNF-α, as a pro-inflammatory cytokine, regulates some physiological and pathological courses. TNF-α level increases in some important diseases such as cancer, arthritis, and diabetes. In addition, it displays an important function in Alzheimer's and cardiovascular diseases. Herein, a novel, sensitive, and selective voltammetric TNF-α immunosensor was prepared by using gold nanoparticles involved in thiol-functionalized multi-walled carbon nanotubes (AuNPs/S-MWCNTs) as sensor platform and bimetallic Ni/Cu-MOFs as sensor amplification. Firstly, the sensor platform was developed on glassy carbon electrode (GCE) surface by using mixture of thiol-functionalized MWCNTs (S-MWCNTs) and AuNPs. Then, capture TNF-α antibodies were conjugated to sensor platform by amino-gold affinity. After capture TNF-α antibodies' immobilization, a new-type voltammetric TNF-α immunosensor was developed by immune reaction between AuNPs/S-MWCNTs immobilized with primer TNF-α antibodies and bimetallic Ni/Cu-MOFs conjugated with seconder TNF-α antibodies. The prepared TNF-α immunosensor was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), x-ray diffraction (XRD) method, x-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM), thermogravimetric analysis, Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). A linearity range of 0.01-1.0 pg mL-1 and a low detection limit of 2.00 fg mL-1 were also obtained for analytical applications.


Assuntos
Técnicas Biossensoriais/métodos , Ouro/química , Nanopartículas Metálicas/química , Nanotubos de Carbono/química , Compostos de Sulfidrila/química , Fator de Necrose Tumoral alfa/sangue , Anticorpos Imobilizados/química , Cobre/química , Técnicas Eletroquímicas/métodos , Humanos , Imunoensaio/métodos , Limite de Detecção , Níquel/química , Fator de Necrose Tumoral alfa/análise
6.
Phys Chem Chem Phys ; 23(22): 12807-12821, 2021 Jun 09.
Artigo em Inglês | MEDLINE | ID: mdl-34059859

RESUMO

Biomass-derived carbonaceous materials have been deemed to be one of the up-and-coming electrode materials for high-performance energy storage systems due to their cost-neutral abundant resources, sustainable nature, easy synthesis methods, and environmentally benign features. In this work, various graphene-like porous carbon networks (GPCs) with three-dimensional (3D) hierarchically ordered "ion highways" have been synthesized by the carbonization/activation of orange-peel wastes for use as an electrode material in high-energy supercapacitors. The porous structures and surface morphologies of the GPCs were rationally fine-tuned as a function of the activation agent ratio. The prepared GPCs offered superior specific surface area in addition to a 3D porous structure with a fine-tuned pore size distribution. The electrochemical behaviors of all the GPCs were evaluated in 6.0 M KOH aqueous electrolyte via a three-electrode electrochemical setup. Owing to their synergistic characteristics, including superior specific surface area (1150 m2 g-1), large pore volume, and fine-tuned 3D porous architecture, GPC-3.0 (synthesized with a KOH : GPC ratio of 3.0, by wt.) exhibited the best capacitive behavior amongst the studied GPCs. The 3D hierarchically ordered architecture acts like well-designed ion highways that boost electron transportation, thereby enhancing electrochemical energy storage. A coin-cell-type symmetrical supercapacitor based on GPC-3.0 was tested in both 1.0 M Na2SO4 (salt-in-water) and 12.0 m NaNO3 (water-in-salt) electrolytes. The supercapacitor cell based on the water-in-salt electrolyte offered a wide operating voltage of 2.3 V. The obtained energy density and power density values were comparable to those of commercial high-performance electrical double-layer capacitors. Such notable findings will shed light on next-generation high-rate electrochemical energy storage systems based on biomass-derived carbonaceous materials.

7.
Mikrochim Acta ; 188(6): 182, 2021 05 07.
Artigo em Inglês | MEDLINE | ID: mdl-33959811

RESUMO

Acute myocardial infarction (AMI) is a significant health problem owing to its high mortality rate. Heart-type fatty acid-binding protein (h-FABP) is an important biomarker in the diagnosis of AMI. In this work, an electrochemical h-FABP immunosensor was developed based on Cd0.5Zn0.5S/d-Ti3C2Tx MXene (MXene: Transition metal carbide or nitride) composite as signal amplificator and core-shell high-crystalline graphitic carbon nitride@carbon dots (hc-g-C3N4@CDs) as electrochemical sensor platform. Firstly, a facile calcination technique was applied to the preparation of hc-g-C3N4@CDs and immobilization of primary antibody was performed on hc-g-C3N4@CDs surface. Then, the conjugation of the second antibody to Cd0.5Zn0.5S/d-Ti3C2Tx MXene was carried out by strong π-π and electrostatic interactions. The prepared electrochemical h-FABP immunosensor was characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), x-ray diffraction (XRD) method, Fourier-transform infrared spectroscopy (FTIR), x-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS). The prepared electrochemical h-FABP immunosensor indicated a good sensitivity with detection limit (LOD) of 3.30 fg mL-1 in the potential range +0.1 to +0.5 V. Lastly, low-cost, satisfactory stable, and environmentally friendly immunosensor was presented for the diagnosis of acute myocardial infarction.


Assuntos
Proteína 3 Ligante de Ácido Graxo/sangue , Grafite/química , Imunoensaio/métodos , Compostos de Nitrogênio/química , Pontos Quânticos/química , Doença Aguda , Anticorpos Imobilizados/imunologia , Biomarcadores/sangue , Cádmio/química , Técnicas Eletroquímicas/métodos , Proteína 3 Ligante de Ácido Graxo/imunologia , Humanos , Limite de Detecção , Infarto do Miocárdio/sangue , Infarto do Miocárdio/diagnóstico , Reprodutibilidade dos Testes , Enxofre/química , Titânio/química , Zinco/química
8.
Mikrochim Acta ; 189(1): 24, 2021 12 11.
Artigo em Inglês | MEDLINE | ID: mdl-34894290

RESUMO

A novel molecularly imprinted electrochemical biosensor for glucose detection is reported based on a hierarchical N-rich carbon conductive-coated TNO structure (TNO@NC). Firstly, TNO@NC was fabricated by a novel polypyrrole-chemical vapor deposition (PPy-CVD) method with minimal waste generation. Afterward, the electrode modification with TNO@NC was performed by dropping TNO@NC particles on glassy carbon electrode surfaces by infrared heat lamp. Finally, the glucose-imprinted electrochemical biosensor was developed in presence of 75.0 mM pyrrole and 25.0 mM glucose in a potential range from + 0.20 to + 1.20 V versus Ag/AgCl via cyclic voltammetry (CV). The physicochemical and electrochemical characterizations of the fabricated molecularly imprinted biosensor was conducted by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD) method, X-ray photoelectron spectroscopy (XPS), electrochemical impedance spectroscopy (EIS), and CV techniques. The findings demonstrated that selective, sensitive, and stable electrochemical signals were proportional to different glucose concentrations, and the sensitivity of molecularly imprinted electrochemical biosensor for glucose detection was estimated to be 18.93 µA µM-1 cm-2 (R2 = 0.99) at + 0.30 V with the limit of detection (LOD) of 1.0 × 10-6 M. Hence, it can be speculated that the fabricated glucose-imprinted biosensor may be used in a multitude of areas, including public health and food quality.


Assuntos
Técnicas Biossensoriais/métodos , Glicemia/análise , Carbono/química , Nióbio/química , Óxidos/química , Titânio/química , Técnicas Biossensoriais/instrumentação , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Eletrodos , Humanos , Limite de Detecção , Impressão Molecular , Porosidade , Reprodutibilidade dos Testes
9.
Mikrochim Acta ; 188(12): 425, 2021 11 23.
Artigo em Inglês | MEDLINE | ID: mdl-34812927

RESUMO

A sensitive and fast sandwich-type electrochemical SARS-CoV­2 (COVID-19) nucleocapsid protein immunosensor was prepared based on bismuth tungstate/bismuth sulfide composite (Bi2WO6/Bi2S3) as electrode platform and graphitic carbon nitride sheet decorated with gold nanoparticles (Au NPs) and tungsten trioxide sphere composite (g-C3N4/Au/WO3) as signal amplification. The electrostatic interactions between capture antibody and Bi2WO6/Bi2S3 led to immobilization of the capture nucleocapsid antibody. The detection antibody was then conjugated to g-C3N4/Au/WO3 via the affinity of amino-gold. After physicochemically characterization via transmission electron microscopy (TEM), scanning electron microscopy (SEM), x-ray diffraction (XRD), and x-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), differential pulse voltammetry (DPV), and electrochemical impedance spectroscopy (EIS) analysis were implemented to evaluate the electrochemical performance of the prepared immunosensor. The detection of SARS-CoV-2 nucleocapsid protein (SARS-CoV-2 NP) in a small saliva sample (100.0 µL) took just 30 min and yielded a detection limit (LOD) of 3.00 fg mL-1, making it an effective tool for point-of-care COVID-19 testing.


Assuntos
Técnicas Eletroquímicas , SARS-CoV-2 , Técnicas Biossensoriais , Ouro , Nanopartículas Metálicas
10.
Foods ; 13(5)2024 Mar 06.
Artigo em Inglês | MEDLINE | ID: mdl-38472923

RESUMO

Dimethoate (DIM) as an organophosphorus pesticide is widely utilized especially in the cultivation of vegetables and fruits due to its killing effect on harmful insects. However, unconscious use of DIM in large amounts can also cause serious health problems. For these reasons, rapid and reliable detection of DIM from food samples is significant. In this study, a novel quartz crystal microbalance (QCM) sensor based on erbium molybdate incorporating sulfur-doped graphitic carbon nitride (EM/S-g-C3N4) and a molecularly imprinting polymer (MIP) was designed for DIM detection in apple juice samples. Firstly, an EM/S-g-C3N4 nanocomposite with high purity was prepared under hydrothermal conditions at high temperatures over a long period of time. After the modification of the EM/S-g-C3N4 nanocomposite on a QCM chip, the polymerization solution including N,N'-azobisisobutyronitrile (AIBN) as an initiator, ethylene glycol dimethacrylate (EGDMA) as a cross-linker, methacryloylamidoglutamic acid (MAGA) as a monomer, and DIM as an analyte was prepared. Then, the polymerization solution was dropped on an EM/S-g-C3N4 nanocomposite modified QCM chip and an ultraviolet polymerization process was applied for the formation of the DIM-imprinted polymers on the EM/S-g-C3N4 nanocomposite modified QCM chip. After the polymerization treatment, some characterization studies, including electrochemical, microscopic, and spectroscopic methods, were performed to illuminate the surface properties of the nanocomposite and the prepared QCM sensor. The values of the limit of quantification (LOQ) and the detection limit (LOD) of the prepared QCM sensor were as 1.0 × 10-9 M and 3.3 × 10-10 M, respectively. In addition, high selectivity, stability, reproducibility, and repeatability of the developed sensor was observed, providing highly reliable analysis results. Finally, thanks to the prepared sensor, it may be possible to detect pesticides from different food and environmental samples in the future.

11.
Biosensors (Basel) ; 14(7)2024 Jul 03.
Artigo em Inglês | MEDLINE | ID: mdl-39056605

RESUMO

In this work, a new surface plasmon resonance (SPR) sensor based on sulphur-doped titanium dioxide (S-TiO2) nanostructures and molecularly imprinted polymer (MIP) was presented for thiram (THI) determination in milk samples. Firstly, the S-TiO2 nanomaterial with a high product yield was prepared by using a facile sol-gel hydrolysis technique with a high product yield. After that, UV polymerization was carried out for the preparation of the THI-imprinted SPR chip based on S-TiO2 using a mixture including ethylene glycol dimethacrylate (EGDMA) as the cross-linker, N,N'-azobisisobutyronitrile (AIBN) as the initiator, and methacryloylamidoglutamicacid (MAGA) as the monomer. The reliability of the sensor preparation procedure has been successfully proven by characterization studies of the prepared nanomaterials and SPR chip surfaces through spectroscopic, microscopic, and electrochemical methods. As a result, the prepared SPR sensor showed linearity in the range of 1.0 × 10-9-1.0 × 10-7 M with a detection limit (LOD) of 3.3 × 10-10 M in the real samples, and a sensor technique for THI determination with high sensitivity, repeatability, and selectivity can be included in the literature.


Assuntos
Leite , Polímeros Molecularmente Impressos , Enxofre , Ressonância de Plasmônio de Superfície , Tiram , Titânio , Titânio/química , Leite/química , Enxofre/química , Polímeros Molecularmente Impressos/química , Animais , Tiram/análise , Limite de Detecção , Impressão Molecular , Polímeros/química
12.
Biosensors (Basel) ; 13(8)2023 Jul 26.
Artigo em Inglês | MEDLINE | ID: mdl-37622846

RESUMO

A novel electrochemical sensor based on MnCO3 nanostructures incorporated into carbon fibers (MnCO3NS/CF), including a molecularly imprinting polymer (MIP), was developed for the determination of Ochratoxin A (OTA). In this study, a sensitive and selective sensor design for OTA detection was successfully performed by utilizing the selectivity and catalysis properties of MIP and the synthesized MnCO3NS/CF material at the same time. MnCO3 nanostructures incorporated into carbon fibers were first characterized by using various analytical techniques. The sensor revealed a linearity towards OTA in the range of 1.0 × 10-11-1.0 × 10-9 mol L-1 with a detection limit (LOD) of 2.0 × 10-12 mol L-1. The improved electrochemical signal strategy was achieved by high electrical conductivity on the electrode surface, providing fast electron transportation. In particular, the analysis process could be finished in less than 5.0 min without complex and expensive equipment. Lastly, the molecular imprinted electrochemical sensor also revealed superior stability, repeatability and reproducibility.


Assuntos
Malus , Nanoestruturas , Fibra de Carbono , Polímeros , Reprodutibilidade dos Testes
13.
Biosensors (Basel) ; 13(7)2023 Jul 12.
Artigo em Inglês | MEDLINE | ID: mdl-37504124

RESUMO

A molecular imprinted electrochemical sensor based on boron-functionalized graphitic carbon nitride (B-g-C3N4) and graphene quantum dots (GQDs) was presented for selective determination of bisphenol A (BPA). In particular, by combining the selectivity and high stability properties, which are the most important advantages of molecular imprinted polymers, and the highly sensitive properties of GQDs/B-g-C3N4 nanocomposite, a highly selective and sensitive analytical method was developed for BPA analysis. Firstly, GQDs/B-g-C3N4 nanocomposite was characterized by using microscopic, spectroscopic, and electrochemical techniques. This novel molecular imprinted electrochemical sensor for BPA detection demonstrated a linearity of 1.0 × 10-11-1.0 × 10-9 M and a low detection limit (LOD, 3.0 × 10-12 M). BPA-imprinted polymer on GQDs/B-g-C3N4 nanocomposite also showed good stability, repeatability and selectivity in food samples.


Assuntos
Técnicas Biossensoriais , Grafite , Impressão Molecular , Pontos Quânticos , Grafite/química , Pontos Quânticos/química , Boro , Impressão Molecular/métodos , Técnicas Biossensoriais/métodos , Limite de Detecção , Polímeros/química , Técnicas Eletroquímicas/métodos
14.
Anal Methods ; 15(15): 1932-1938, 2023 04 13.
Artigo em Inglês | MEDLINE | ID: mdl-37013684

RESUMO

5-Hydroxymethyl furfural (HMF) is an intermediate produced by dehydrating sugars, such as fructose, sucrose, and glucose, in an acidic medium or during the Maillard reaction. It also occurs due to the storage of sugary foods at inappropriate temperatures. In addition, HMF is seen as a quality criterion in products. In this study, a novel molecularly imprinted electrochemical sensor based on graphene quantum dots incorporated NiAl2O4 (GQDs-NiAl2O4) nanocomposite was presented for the selective determination of HMF in coffee samples. Various microscopic, spectroscopic, and electrochemical methods were carried out for the structural characterizations of GQDs-NiAl2O4 nanocomposite. The molecularly imprinted sensor was prepared by multi-scanning using cyclic voltammetry (CV) in the presence of 100.0 mM pyrrole monomer and 25.0 mM HMF. After method optimization, the sensor revealed linearity towards HMF in the range of 1.0-10.0 ng L-1 with a detection limit (LOD) of 0.30 ng L-1. The developed MIP sensor's high repeatability, selectivity, stability, and fast response ability can provide reliable HMF detection in beverages, such as coffee, which is heavily consumed.


Assuntos
Grafite , Impressão Molecular , Nanocompostos , Pontos Quânticos , Café , Grafite/química , Impressão Molecular/métodos , Nanocompostos/química , Pontos Quânticos/química , Compostos de Alumínio/química
15.
Micromachines (Basel) ; 15(1)2023 Dec 19.
Artigo em Inglês | MEDLINE | ID: mdl-38276834

RESUMO

This research attempt involved the development and utilization of a newly designed surface plasmon resonance (SPR) sensor which incorporated sulfur-doped graphitic carbon nitride (S-g-C3N4) as the molecular imprinting material. The primary objective was to employ this sensor for the quantitative analysis of Fenpicoxamid (FEN) in rice samples. The synthesis of S-g-C3N4 with excellent purity was achieved using the thermal poly-condensation approach, which adheres to the principles of green chemistry. Afterwards, UV polymerization was utilized to fabricate a surface plasmon resonance (SPR) chip imprinted with FEN, employing S-g-C3N4 as the substrate material. This process involved the inclusion of N,N'-azobisisobutyronitrile (AIBN) as the initiator, ethylene glycol dimethacrylate (EGDMA) as the cross-linker, methacryloylamidoglutamic acid (MAGA) as the monomer, and FEN as the analyte. After successful structural analysis investigations on a surface plasmon resonance (SPR) chip utilizing S-g-C3N4, which was imprinted with FEN, a comprehensive investigation was conducted using spectroscopic, microscopic, and electrochemical techniques. Subsequently, the kinetic analysis applications, namely the determination of the limit of quantification (LOQ) and the limit of detection (LOD), were carried out. For analytical results, the linearity of the FEN-imprinted SPR chip based on S-g-C3N4 was determined as 1.0-10.0 ng L-1 FEN, and LOQ and LOD values were obtained as 1.0 ng L-1 and 0.30 ng L-1, respectively. Finally, the prepared SPR sensor's high selectivity, repeatability, reproducibility, and stability will ensure safe food consumption worldwide.

16.
Anal Chim Acta ; 1200: 339609, 2022 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-35256133

RESUMO

Small cell lung cancer (SCLC) is highly associated with the risk of early metastasis. Neuron-specific enolase (NSE), a biomarker of SCLC, is directly related to tumor burden and early diagnosis. This biomarker exists in nerve tissue and neuroendocrine tissue. In this study, an electrochemical NSE immunosensor based on gold nanoparticles modified molybdenum disulfide and reduced graphene oxide (AuNPs@MoS2/rGO) as the electrode platform and CoFe2O4@Ag nanocomposite as the signal amplification was developed. The immobilization of anti-NSE capture antibody was successfully performed on AuNPs@MoS2/rGO modified electrode surface by amino-gold affinity and the conjugation of anti-NSE secondary antibody on CoFe2O4@Ag nanocomposite was successfully completed by the strong esterification reaction. The final immunosensor was designed by the specific interactions of electrode platform and signal amplification. The fabricated nanocomposites and electrochemical immunosensor were characterized by both physicochemical characterization techniques including transmission electron microscopy (TEM), scanning electron microscopy (SEM), x-ray diffraction (XRD), x-ray photoelectron spectroscopy (XPS), fourier transform infrared spectroscopy (FTIR), and electrochemical methods such as cyclic voltammetry (CV), square wave voltammetry (SWV), and electrochemical impedance spectroscopy (EIS). The quantification limit (LOQ) and the determination limit (LOD) were computed to be 0.01 pg mL-1 and 3.00 fg mL-1, respectively. In brief, it can be speculated that the constructed electrochemical NSE immunosensor can be successfully utilized in the early diagnosis for lung cancer.


Assuntos
Técnicas Biossensoriais , Grafite , Nanopartículas Metálicas , Nanocompostos , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Ouro/química , Grafite/química , Imunoensaio/métodos , Limite de Detecção , Nanopartículas Metálicas/química , Molibdênio/química , Nanocompostos/química , Fosfopiruvato Hidratase
17.
Anal Chim Acta ; 1148: 338202, 2021 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-33516376

RESUMO

Interleukin 6 (IL-6) acts as both a proinflammatory and anti-inflammatory cytokine and is generally utilized as an important diagnostic biomarker for sepsis. In addition, the high levels of IL-6 measured in plasma have been associated with pathological inflammation. A novel quartz crystal microbalance (QCM) immunoassay method was presented for high sensitivity and selectivity detection of interleukin-6 (IL-6) based on gold nanoparticles functionalized sulfur-doped graphene quantum dot (AuNPs/S-GQD) and hollow ZnS-CdS nanocage (h-ZnS-CdS NC). Firstly, AuNPs/S-GQD nanocomposite was synthesized in the presence of tetrachloroauric acid and then conjugated onto anti-IL-6 antibodies by amino-gold affinity. The sandwich-type QCM immunoassay probe was prepared by immune-reaction between AuNPs/S-GQD/QCM immobilized with anti-IL-6 capture antibodies and h-ZnS-CdS NC including detection anti-IL-6 antibodies in the presence of target IL-6. The prepared QCM immunoassay probe was characterized by transmission electron microscopy (TEM), scanning electron microscope (SEM), x-ray diffraction (XRD) method, x-ray photoelectron spectroscopy (XPS), Raman spectroscopy, UV-vis spectroscopy, Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The QCM immunosensor showed a linearity range (0.01-2.0 pg mL-1) and a low detection limit (3.33 fg mL-1). Lastly, high stable and selective QCM immunosensor was applied to prepared plasma samples with good recovery.


Assuntos
Técnicas Biossensoriais , Grafite , Nanopartículas Metálicas , Pontos Quânticos , Anticorpos Imobilizados , Técnicas Eletroquímicas , Ouro , Imunoensaio , Interleucina-6 , Limite de Detecção , Sulfetos , Enxofre , Compostos de Zinco
18.
Nanoscale ; 13(8): 4660-4669, 2021 Mar 04.
Artigo em Inglês | MEDLINE | ID: mdl-33620353

RESUMO

Lung cancer is one of deadliest and most life threatening cancer types. Cytokeratin 19 fragment antigen 21-1 (CYFRA 21-1) is a significant biomarker for the diagnosis of non-small cell lung cancer (NSCLC). Due to these reasons, a novel electrochemical immunosensor based on a silicon nitride (Si3N4)-molybdenum disulfide (MoS2) composite on multi-walled carbon nanotubes (Si3N4/MoS2-MWCNTs) as an electrochemical sensor platform and core-shell type magnetic mesoporous silica nanoparticles@gold nanoparticles (MMSNs@AuNPs) as a signal amplifier was presented for CYFRA21-1 detection in this study. Capture antibody (Ab1) immobilization on a Si3N4/MoS2-MWCNT modified glassy carbon electrode (Si3N4/MoS2-MWCNTs/GCE) was firstly successfully performed by stable electrostatic/ionic interactions between the -NH2 groups of the capture antibody and the polar groups of Si3N4/MoS2. Then, specific antibody-antigen interactions between the electrochemical sensor platform and the signal amplifier formed a novel voltammetric CYFRA21-1 immunosensor. The prepared composite materials and electrochemical sensor surfaces were characterized by transmission electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). A linearity range of 0.01-1.0 pg mL-1 and a low detection limit (LOD) of 2.00 fg mL-1 were also obtained for analytical applications. Thus, the proposed immunosensor based on Si3N4/MoS2-MWCNTs and MMSNs@AuNPs has great potential for medical diagnosis of lung cancer.


Assuntos
Técnicas Biossensoriais , Carcinoma Pulmonar de Células não Pequenas , Neoplasias Pulmonares , Nanopartículas de Magnetita , Nanopartículas Metálicas , Nanotubos de Carbono , Antígenos de Neoplasias , Biomarcadores Tumorais , Técnicas Eletroquímicas , Eletrodos , Ouro , Humanos , Imunoensaio , Queratina-19 , Limite de Detecção , Pulmão , Neoplasias Pulmonares/diagnóstico , Molibdênio
19.
J Colloid Interface Sci ; 592: 174-185, 2021 Jun 15.
Artigo em Inglês | MEDLINE | ID: mdl-33662823

RESUMO

Organophosphorus insecticide fenamiphos (FEN) is utilized to control the detrimental nematode pests. In this report, a novel molecular imprinted electrochemical sensor for insecticide FEN detection was prepared. The molecular imprinted sensor was prepared based on Co3O4 nanowire and core-shell Co3O4@MOF-74 nanocomposite. Firstly, hydrothermal method followed by thermal annealing was applied for the preparation of Co3O4 nanowire. Then, solvothermal technique was used in no presence of metal salts to prepare core-shell Co3O4@MOF-74 nanocomposite. In addition, several solvothermal cycles were tried to optimally adjust the reaction efficiency. After the modification of the clean carbon electrode surfaces with Co3O4@MOF-74 nanocomposites, the molecular imprinted electrodes based on Co3O4@MOF-74 nanocomposites were prepared in presence of 100.0 mM pyrrole as monomer and 25.0 mM FEN as analyte molecule between +0.30 V and +1.50 V by cyclic voltammetry (CV). The prepared molecularly imprinted sensor based on Co3O4 nanowire and core-shell Co3O4@MOF-74 nanocomposite was characterized by transmission electron microscopy (TEM), scanning electron microscope (SEM), x-ray diffraction (XRD) method, x-ray photoelectron spectroscopy (XPS), fourier transform infrared spectroscopy (FTIR), electrochemical impedance spectroscopy (EIS) and CV. The quantification limit (LOQ) and the detection limit (LOD) were obtained as 1.0 × 10-11 M and 3.0 × 10-12 M, respectively, by using the developed sensor. Hence, the developed molecularly imprinting electrochemical sensor having high selectivity, stability and reproducibility was presented in this study for insecticide FEN detection.

20.
Acta Chim Slov ; 57(1): 212-21, 2010 Mar.
Artigo em Inglês | MEDLINE | ID: mdl-24061675

RESUMO

In this work we report the synthesis of two novel square-planar copper(II) complexes, namely, (2-aminomethylpyridinium-pyridinedicarboxylato)copper(II) dihydrate, [Cu(pydc)(2-amp)] • 2H2O (1) and (8-hydroxyquinolinum-pyridinedicarboxylato)copper(II) hydrate, [Cu(pydc)(8-HQ)] • H2O (2) (2-amp = 2-aminomethylpyridine, 8-HQ = 8-hydroxyquinoline, H2pydc = pyridine-2,5-dicarboxylic acid or isocinchomeronic acid) and present the first preliminary study on kinetics and biological activities of copper complexes. The synthesized complexes have been characterized by elemental, spectroscopic (FT-IR, UV and mass spectra), thermal analysis, magnetic and conductivity measurements techniques. Kinetic parameters were obtained for each stage of thermal degradation of the complexes using Coats-Redfern and Horowitz-Metzger methods. Antimicrobial activities of two complexes and two ligands were evaluated using agar diffusion method. Antimicrobial activity of complex 2 was determined with the agar dilution methods. The results were compared with two well known antibiotics, namely, tetracycline and nystatin.

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