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1.
Talanta ; 277: 126330, 2024 May 27.
Artigo em Inglês | MEDLINE | ID: mdl-38833905

RESUMO

In this work, flower-like ZnO nanoparticles (ZnONPs) were synthesized using zinc nitrate (Zn(NO3)2 6H2O) as a precursor with KOH. The morphology of the ZnONPs was controlled by varying the synthesis temperature at 50, 75 and 95 °C. The morphology and structure of ZnONPs were characterized using Scanning Electron Microscopy, and X-Ray Diffraction and Brunauer-Emmett Teller analysis. ZnONPs were successfully synthesized by a simple chemical precipitation method. A synthesis temperature of 75 °C produced the most suitable flower-like ZnONPs, which were combined with graphene nanoplatelets to develop a label-free electrochemical immunosensor for the detection of the colon cancer biomarker carcinoembryonic antigen in human serum. Under optimum conditions, the developed immunosensor showed a linear range of 0.5-10.0 ng mL-1 with a limit of detection of 0.44 ng mL-1. The label-free electrochemical immunosensor exhibited good selectivity, reproducibility, and repeatability, and recoveries were excellent. The immunosensor is used with a Near-Field Communication potentiostat connected to a smartphone to facilitate point-of-care cancer detection in low-resource locations.

2.
Talanta ; 278: 126446, 2024 Jun 26.
Artigo em Inglês | MEDLINE | ID: mdl-38936107

RESUMO

The simultaneous synthesis of gold nanoparticles (AuNPs) and graphene by laser ablation was demonstrated. The in-situ synthesis was performed by laser ablation of a polymer substrate covered with a gold precursor dispersion. The gold precursor was prepared in a copolymer solution of pyrrole (Py) and chitosan (Chi) to improve the nucleation of gold embedded on the laser-induced graphene electrode (LIGE). The morphology of AuNPs-pPy-Chi/LIGE was studied by scanning electron microscopy and characterized electrochemically by cyclic voltammetry. A comprehensive investigation of the electrochemical and physical features of the AuNPs-pPy-Chi/LIGE was carried out. The parameters of differential pulse voltammetry were adjusted to enhance the response to ascorbic acid (AA). The AuNPs-pPy-Chi/LIGE produced two linear ranges: from 0.25 to 5.00 and 5.00-25.00 mmol L-1. The limit of detection was 0.22 mmol L-1. Hundreds of electrodes were tested to demonstrate the excellent reproducibility of the AuNPs-pPy-Chi/LIGE fabrication. Overall, the proposed electrode allows the successful detection of AA in orange juice products with acceptable accuracy (recoveries = 97 ± 2 to 109.1 ± 0.7). The preparation strategy of the proposed AuNPs-pPy-Chi/LIGE could be adapted to detect other compounds or biomarkers.

3.
Food Chem ; 447: 138987, 2024 Jul 30.
Artigo em Inglês | MEDLINE | ID: mdl-38518621

RESUMO

Nitrite (NO2-) is widely used as an additive to extend the shelf life of food products. Excessive nitrite intake not only causes blood-related diseases but also has the potential risk of causing cancers. A disposable screen-printed electrode was modified with nano­palladium decorated bismuth sulfide microspheres (nanoPd@Bi2S3MS/SPE), and integrated with a smartphone-interfaced potentiostat to develop a portable, electrochemical nitrite sensor. NanoPd@Bi2S3MS was prepared by the hydrothermal reduction of a Bi2S3MS and Pd2+ dispersion and drop cast on the SPE. The nanoPd@Bi2S3MS/SPE was coupled with a smartphone-controlled portable potentiostat and applied to determine nitrite in food samples. The linear range of the sensor was 0.01-500 µM and the limit of detection was 0.0033 µM. The proposed system showed good repeatability, reproducibility, catalytic stability, and immunity to interferences. The proposed electrode material and a smartphone-based small potentiostat created a simple, portable, fast electrochemical sensing system that accurately measured nitrite in food samples.


Assuntos
Bismuto , Nitritos , Paládio , Sulfetos , Microesferas , Smartphone , Reprodutibilidade dos Testes , Eletrodos , Técnicas Eletroquímicas
4.
Talanta ; 272: 125755, 2024 May 15.
Artigo em Inglês | MEDLINE | ID: mdl-38364561

RESUMO

A novel label-free electrochemical immunosensor was prepared for the detection of carbohydrate antigen 19-9 (CA19-9) and carcinoembryonic antigen (CEA) as biomarkers of cholangiocarcinoma (CCA). A nanocomposite of gold nanoparticles, molybdenum trioxide, and chitosan (Au-MoO3-Chi) was layer-by-layer assembled on the porous graphene (PG) modified a dual screen-printed electrode using a self-assembling technique, which increased surface area and conductivity and enhanced the adsorption of immobilized antibodies. The stepwise self-assembling procedure of the modified electrode was further characterized morphologically and functionally. The electroanalytical detection of biomarkers was based on the interaction between the antibody and antigen of each marker via linear sweep voltammetry using ferrocyanide/ferricyanide as an electrochemical redox indicator. Under optimized conditions, the fabricated immunosensor showed linear relationships between current change (ΔI) and antigen concentrations in two ranges: 0.0025-0.1 U mL-1 and 0.1-1.0 U mL-1 for CA19-9, and 0.001-0.01 ng mL-1 and 0.01-1.0 ng mL-1 for CEA. The limits of detection (LOD) were 1.0 mU mL-1 for CA19-9 and 0.5 pg mL-1 for CEA. Limits of quantitation (LOQ) were 3.3 mU mL-1 for CA19-9 and 1.6 pg mL-1 for CEA. The selectivity of the developed immunosensor was tested on mixtures of antigens and was then successfully applied to determine CA19-9 and CEA in human serum samples, producing satisfactory results consistent with the clinical method.


Assuntos
Técnicas Biossensoriais , Colangiocarcinoma , Grafite , Nanopartículas Metálicas , Humanos , Grafite/química , Antígeno Carcinoembrionário , Ouro/química , Técnicas Biossensoriais/métodos , Antígeno CA-19-9 , Sistemas Automatizados de Assistência Junto ao Leito , Porosidade , Nanopartículas Metálicas/química , Imunoensaio/métodos , Eletrodos , Limite de Detecção , Colangiocarcinoma/diagnóstico , Técnicas Eletroquímicas/métodos
5.
Mikrochim Acta ; 190(6): 232, 2023 05 22.
Artigo em Inglês | MEDLINE | ID: mdl-37213023

RESUMO

A simple label-free electrochemical immunosensor for ovarian cancer (OC) detection was developed using a hierarchical microporous carbon material fabricated from waste coffee grounds (WCG). The analysis method exploited near-field communication (NFC) and a smartphone-based potentiostat. Waste coffee grounds were pyrolyzed with potassium hydroxide and used to modify a screen-printed electrode. The modified screen-printed electrode was decorated with gold nanoparticles (AuNPs) to capture a specific antibody. The modification and immobilization processes were characterized by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The sensor had an effective dynamic range of 0.5 to 50.0 U mL-1 of cancer antigen 125 (CA125) tumor marker with a correlation coefficient of 0.9995. The limit of detection (LOD) was 0.4 U mL-1. A comparison of the results obtained from human serum analysis with the proposed immunosensor and the results obtained from the clinical method confirmed the accuracy and precision of the proposed immunosensor.


Assuntos
Técnicas Biossensoriais , Nanopartículas Metálicas , Neoplasias Ovarianas , Feminino , Humanos , Carbono , Nanopartículas Metálicas/química , Ouro/química , Café , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Imunoensaio/métodos , Neoplasias Ovarianas/diagnóstico
6.
Food Chem ; 421: 136170, 2023 Sep 30.
Artigo em Inglês | MEDLINE | ID: mdl-37087990

RESUMO

Coffee beans can be contaminated during roasting by polycyclic aromatic hydrocarbons (PAHs), some of which have been classified as carcinogens. An extraction device for PAHs in coffee drinks was designed with six compact DC motors rotating six sorbents. The sorbents were plaswood propellers modified by one-step electrodeposition of a poly(ortho-phenylenediamine) and Zn composite (PoPD-Zn). Benzo(a)anthracene (BaA), chrysene (Chry), benzo(b)fluoranthene (BbF), and benzo(a)pyrene (BaP) were chosen as representative PAHs. Scanning electron micrographs of the PoPD-Zn showed a porous structure. The extracted PAHs were quantified by gas chromatography coupled with a flame ionization detector. Detected concentrations of PAHs in coffee drink samples were as follows: BaA 1.4 ± 0.4 to 16.5 ± 0.8 µg L-1; Chry 0.5 ± 0.2 to 2.1 ± 0.5 µg L-1; BbF 2.2 ± 0.6 µg L-1; and BaP 6.2 ± 1.0 µg L-1. Good recoveries ranging from 82.7 ± 1.9% to 99.0 ± 0.5% were obtained.


Assuntos
Hidrocarbonetos Policíclicos Aromáticos , Hidrocarbonetos Policíclicos Aromáticos/análise , Galvanoplastia , Zinco
7.
Talanta ; 255: 124229, 2023 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-36641867

RESUMO

A compact and low-cost multi-electrode array (MEA) is presented, comprising four working electrodes with shared reference and auxiliary electrodes. Prussian blue was electrodeposited on the MEA using chronoamperometry with a positive potential of 0.3 V. Prussian blue nanocubes (PBNCs) were formed, which were observed using scanning electron microscopy. The precision of the four working electrodes was demonstrated using ferric/ferro cyanide (RSD <5.8%). The surface roughness of the working electrodes of the fabricated MEA was investigated by atomic force microscopy and compared with that of a commercial MEA. The PBNCs were the platform for a label-free immunosensor that detected four breast cancer tumor markers (CEA, CA125, CA153, and CA199) using specific antibodies. The processes of antibody immobilization were investigated using cyclic voltammetry and electrochemical impedance spectroscopy. The immunosensor was evaluated using real human serum samples, yielding acceptable recoveries (95.1-104.1%, RSD < 3.9) for the four tumor markers. These findings confirmed that our label-free immunosensor based on PBNCs could be a promising device for point-of-care testing and could pave the way for the establishment of new platforms for the screening of various breast cancer tumor markers.


Assuntos
Técnicas Biossensoriais , Neoplasias da Mama , Humanos , Feminino , Biomarcadores Tumorais , Neoplasias da Mama/diagnóstico , Técnicas Biossensoriais/métodos , Técnicas Eletroquímicas/métodos , Imunoensaio/métodos , Anticorpos , Eletrodos
8.
Talanta ; 254: 124137, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36463801

RESUMO

Insulin is the polypeptide hormone that regulates blood glucose levels. It is used as an indicator of both types of diabetes. An electrochemical insulin sensor was developed using a gold electrode modified with carboxylated multiwalled carbon nanotubes (f-MWCNTs) and molecularly imprinted polymer (MIP) cryogel. The MIP provided specific recognition sites for insulin, while the macropores of the cryogel promoted the mass transfer of insulin to the recognition sites. The f-MWCNTs increased the effective surface area and conductivity of the sensor and also reduced the potential required to oxidize insulin. Insulin oxidation was directly measured in a flow system using square wave voltammetry. This MIP cryogel/f-MWCNTs sensor provided a linear range of 0.050-1.40 pM with a very low limit of detection (LOD) of 33 fM. The sensor exhibited high selectivity and long-term stability over 10 weeks of dry storage at room temperature. The results of insulin determination in human serum using the sensor compared well with the results of the Elecsys insulin assay. The developed MIP sensor offers a promising alternative for the diagnosis and treatment of diabetes.


Assuntos
Diabetes Mellitus , Impressão Molecular , Nanotubos de Carbono , Humanos , Polímeros Molecularmente Impressos , Impressão Molecular/métodos , Insulina , Criogéis , Técnicas Eletroquímicas/métodos , Eletrodos , Limite de Detecção , Diabetes Mellitus/diagnóstico
9.
Talanta ; 254: 124169, 2023 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-36549140

RESUMO

We developed a fully integrated smart sensing device for on-site testing of food to detect trace formaldehyde (FA). A nano-palladium grafted laser-induced graphene (nanoPd@LIG) composite was synthesized by one-step laser irradiation of a Pd2+-chitosan-polyimide precursor. The composite was synthesized in the form of a three-electrode sensor on a polymer substrate. The electrochemical properties and morphology of the fabricated composite were characterized and the electrochemical kinetics of FA oxidation at the nanoPd@LIG electrode were investigated. The nanoPd@LIG electrode was combined with a smart electrochemical sensing (SES) device to determine FA electrochemically. The proposed SES device uses near field communication (NFC) to receive power and transfer data between a smartphone interface and a battery-free sensor. The proposed FA sensor exhibited a linear detection range from 0.01 to 4.0 mM, a limit of detection of 6.4 µM, good reproducibility (RSDs between 2.0 and 10.1%) and good anti-interference properties for FA detection. The proposed system was used to detect FA in real food samples and the results correlated well with the results from a commercial potentiostat and a spectrophotometric analysis.


Assuntos
Grafite , Grafite/química , Paládio/química , Reprodutibilidade dos Testes , Smartphone , Eletrodos , Lasers , Formaldeído , Técnicas Eletroquímicas/métodos
10.
Sensors (Basel) ; 22(8)2022 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-35459019

RESUMO

Multichannel graphite electrodes (MGrEs) have been designed and fabricated in this study. A template was cut from an adhesive plastic sheet using a desktop cutting device. The template was placed on a polypropylene substrate, and carbon graphite ink was applied with a squeegee to the template. The size of the auxiliary electrode (AE) as well as the location of the reference electrode (RE) of MGrEs design were investigated. Scanning electron microscopy was used to determine the thickness of the ink on the four working electrodes (WEs), which was 21.9 ± 1.8 µm. Cyclic voltammetry with a redox probe solution was used to assess the precision of the four WEs. The intra-electrode repeatability and inter-electrode reproducibility of the MGrEs production were satisfied by low RSD (<6%). Therefore, the MGrEs is reliable and capable of detecting four replicates of the target analyte in a single analysis. The electrochemical performance of four WEs was investigated and compared to one WE. The sensitivity of the MGrEs was comparable to the sensitivity of a single WE. The MGrEs' potential applications were investigated by analyzing the nitrite in milk and tap water samples (recoveries values of 97.6 ± 0.4 to 110 ± 2%).


Assuntos
Grafite , Técnicas Eletroquímicas/métodos , Eletrodos , Limite de Detecção , Impressão Tridimensional , Reprodutibilidade dos Testes
11.
Methods Appl Fluoresc ; 10(3)2022 Apr 20.
Artigo em Inglês | MEDLINE | ID: mdl-35442215

RESUMO

This work developed a sensitive DNA-based fluorescent probe comprising a cysteine binding unit and a signal amplification unit based on a catalyzed hairpin assembly (CHA) reaction. The cysteine binding unit comprises a homodimer of single-stranded DNA (ssDNA) rich in cytosine and held together by silver ions. In the presence of cysteine, the homodimer is disintegrated because of cysteine-silver binding that liberates the ssDNA, which drives the CHA reaction in the signal amplification unit. Förster resonance energy transfer (FRET) was used to report the generation of the amplified double-stranded DNA (dsDNA) product. Under the optimal conditions, the probe provided a good linearity (100-1200 nM), a good detection limit (47.8 ± 2.7 nM) and quantification limit (159.3 ± 5.3 nM), and a good sensitivity (1.900 ± 0.045µM-1). The probe was then used to detect cysteine in nine real food supplement samples. All results provided good recoveries that are acceptable by the AOAC, indicating that it has potential for practical applications.


Assuntos
Técnicas Biossensoriais , Transferência Ressonante de Energia de Fluorescência , Técnicas Biossensoriais/métodos , Catálise , Cisteína , DNA/genética , DNA de Cadeia Simples , Corantes Fluorescentes , Prata
12.
Mikrochim Acta ; 188(12): 415, 2021 11 09.
Artigo em Inglês | MEDLINE | ID: mdl-34755233

RESUMO

Noninvasive diagnosis using salivary samples to detect thiocyanate provides vital information on individual health. This article demonstrates the first example of a wearable sensing device to noninvasively assess thiocyanate levels. The customized screen-printed electrode system is integrated into a form of a mouthguard squarewave-voltammetric sensor toward the convenient and fast detection of the salivary biomarker within 15 s. The sensor with a protective film to mitigate the effect of biofouling offers high sensitivity and selectivity toward the detection of thiocyanate ions. Partial least square regression is applied to analyze the high-order squarewave-voltammetric data over the applied potential range of 0-1.75 V vs Ag/AgCl and quantify the thiocyanate concentration in a complex matrix. The mouthguard sensor operating under physiological conditions can monitor a wide range of thiocyanate (up to 11 mM) with a low detection limit of 30 µM. The demonstration introduces a unique approach, that obviates the requirement for blood sampling, to study thiocyanate levels of healthy people, cigarette smokers, or people with other health conditions. It is envisioned that the new cavitas device possesses a substantial promise for diverse biomedical diagnosis applications.


Assuntos
Técnicas Biossensoriais/instrumentação , Técnicas Eletroquímicas/instrumentação , Saliva/química , Tiocianatos/química , Dispositivos Eletrônicos Vestíveis , Biomarcadores/análise , Cianetos/química , Cianetos/toxicidade , Eletrodos , Exposição Ambiental , Humanos , Monitorização Fisiológica
13.
Talanta ; 224: 121787, 2021 Mar 01.
Artigo em Inglês | MEDLINE | ID: mdl-33379016

RESUMO

A highly sensitive and selective label-free electrochemical immunosensor was successfully fabricated for measuring prostate-specific antigen (PSA). A composite of chitosan, graphene, ionic liquid and ferrocene (CS-GR-IL-Fc) was drop casted onto a screen-printed carbon electrode (SPCE) and frozen to create a layer of 3D porous cryogel (CS-GR-IL-Fc cry) which was decorated with gold nanoparticles (AuNPs). The biocompatibility and porosity of the cryogel increased the surface area available for AuNPs loading via amino groups and the population of anti-PSA, immobilized on the AuNPs via chemisorption, could be increased. The CS-GR-IL-Fc cry displayed excellent conductivity, enhancing electron transfer and amplifying the current signal. Differential pulse voltammetry was employed to determine PSA by measuring the reduction in the Fc oxidation peak current in response to the formation of PSA/anti-PSA immunocomplex. Under the optimized incubation time and electrolyte pH, the developed immunosensor displayed excellent analytical performances, including a wide linear range at concentrations from 1.0 × 10-7 to 1.0 × 10-1 ng mL-1, with a very low limit of detection of 4.8 × 10-8 ng mL-1 and good reproducibility (relative standard deviation of <4.6%, n = 6), stability (90% sensitivity within 20 days), repeatability (12 cycles of binding-rebinding, the sensitivity > 90%) and selectivity. The results obtained from the device for the determination of PSA in human serum were consistent with results from the enzyme-linked immunosorbent assay (P > 0.05), and indicated the promising potential of the proposed immunosensor in clinical diagnosis.


Assuntos
Técnicas Biossensoriais , Quitosana , Grafite , Líquidos Iônicos , Nanopartículas Metálicas , Nanocompostos , Criogéis , Técnicas Eletroquímicas , Ouro , Humanos , Imunoensaio , Masculino , Metalocenos , Porosidade , Antígeno Prostático Específico , Reprodutibilidade dos Testes
14.
Food Chem ; 342: 128336, 2021 Apr 16.
Artigo em Inglês | MEDLINE | ID: mdl-33077280

RESUMO

Polypyrrole magnetic microspheres were synthesized and used to extract carbaryl, carbofuran, and methomyl before analysis by a high-performance liquid chromatography with diode array detection. Under optimal conditions, four times the preconcentration was achieved with the use of only 1.2 mL of sample. Good linearity with ranges of 3.0-7.5 × 103, 6.0-4.5 × 103, and 15-3.0 × 103 ng kg-1 and limits of detection of 1.37 ± 0.10, 4.7 ± 1.2, and 10.1 ± 5.7 ng kg-1 were obtained, respectively. Good reproducibility (RSDs < 5%) was achieved over 24 cycles of extraction and regeneration. Good accuracy (recoveries 81.6 ± 1.5%-108.3 ± 2.2%) and good precision (RSDs 0.11%-4.5%) were obtained. Carbaryl was detected in apple (2.75 ± 0.23 ng kg-1), carbofuran in tomato (11.34 ± 0.61 ng kg-1), and methomyl in watermelon (34.7 ± 1.7 ng kg-1). The relative expanded uncertainty of the measurement method was less than 14% for all three pesticides.


Assuntos
Carbonato de Cálcio/química , Carbamatos/isolamento & purificação , Citrullus/química , Imãs/química , Microesferas , Praguicidas/isolamento & purificação , Solanum lycopersicum/química , Carbamatos/química , Técnicas de Química Sintética , Limite de Detecção , Praguicidas/química , Polímeros/química , Pirróis/química , Reprodutibilidade dos Testes
15.
Anal Chim Acta ; 1130: 60-71, 2020 Sep 15.
Artigo em Inglês | MEDLINE | ID: mdl-32892939

RESUMO

A novel multiplexed label-free electrochemical immunosensor was fabricated using graphene/methylene blue-chitosan/antibody and bovine serum albumin on indium tin oxide glass electrode for the simultaneous determination of three types of tumor markers including carcinoembryonic antigen (CEA), cancer antigens 153 (CA153), and cancer antigen 125 (CA125). Cyclic voltammetry, electrochemical impedance spectroscopy, and scanning electron microscopy were employed to monitor each fabrication step. Under the optimized experiment conditions, the immunosensor exhibited good reproducibility and selectivity with linear ranges of 0.10-1.00 pg mL-1 and 1.00-100.00 pg mL-1 for CEA, 0.10-2.50 mU mL-1 and 2.50-100.00 mU mL-1 for CA153, 0.10-2.50 mU mL-1 and 2.50-100.00 mU mL-1 for CA125, a detection limit of 0.04 pg mL-1 for CEA, 0.04 mU mL-1 for CA153, and 0.04 mU mL-1 for CA125. This electrochemical immunosensor was successfully applied to detect three tumor markers in blood serum samples with good recoveries. The reliability of the electrochemical immunosensor to detect three tumor markers in blood serum samples was in good agreement (P > 0.05) with that of the enzyme-linked fluorescent assay method.


Assuntos
Técnicas Biossensoriais , Neoplasias da Mama , Anticorpos Imobilizados , Neoplasias da Mama/diagnóstico , Antígeno Carcinoembrionário , Técnicas Eletroquímicas , Eletrodos , Ouro , Humanos , Imunoensaio , Limite de Detecção , Medicina de Precisão , Reprodutibilidade dos Testes
16.
J Environ Sci Health B ; 55(1): 60-68, 2020.
Artigo em Inglês | MEDLINE | ID: mdl-31971076

RESUMO

This work reports the development of a very-simple-to-construct stir-bar extraction device so called "a dumbbell-shaped stainless steel stir-bar." The extraction device was assembled from a rolled up stainless steel net filled with an XAD-2 sorbent and a metal rod to allow the use of a magnetic stirrer during extraction. The dumbbell-shaped stainless steel stir-bar was used to extract diethyl phthalate (DEP), dibutyl phthalate (DBP), and di(2-ethylhexyl) phthalate (DEHP) before analysis by a gas chromatograph equipped with an electron capture detector (GD-ECD). Under the optimal conditions, the developed method provided a good linearity from 10.0 to 1,000.0 ng mL-1 for all three compounds. Limits of detection and limits of quantification were 9.37 ± 0.29 ng mL-1 and 31.22 ± 0.95 ng mL-1 for DEP, 5.73 ± 0.31 ng mL-1 and 19.1 ± 1.0 ng mL-1 for DBP and 3.30 ± 0.06 ng mL-1 and 11.0 ± 0.19 ng mL-1 for DEHP, respectively. Good recoveries in the range of 81.89 ± 0.17 to 109.5 ± 2.0% were achieved when the method was used to extract phthalate esters in five instant noodle and two rice soup samples.


Assuntos
Fracionamento Químico/instrumentação , Análise de Alimentos/instrumentação , Oryza , Ácidos Ftálicos/isolamento & purificação , Aço Inoxidável , Fracionamento Químico/métodos , Cromatografia Gasosa , Dibutilftalato/isolamento & purificação , Dietilexilftalato/isolamento & purificação , Desenho de Equipamento , Análise de Alimentos/métodos , Contaminação de Alimentos/análise , Limite de Detecção , Ácidos Ftálicos/química , Reprodutibilidade dos Testes
17.
Talanta ; 188: 658-664, 2018 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-30029427

RESUMO

This article reports the detection of Salmonella spp. based on M13 bacteriophage in a capacitive flow injection system. Salmonella-specific M13 bacteriophage was immobilized on a polytyramine/gold surface using glutaraldehyde as a crosslinker. The M13 bacteriophage modified electrode can specifically bind to Salmonella spp. via the amino acid groups on the filamentous phage. An alkaline solution was used to break the binding between the sensing surface and the analyte to allow renewable use up to 40 times. This capacitive system provided good reproducibility with a relative standard deviation (RSD) of 1.1%. A 75 µL min-1 flow rate and a 300 µL sample volume provided a wide linear range, from 2.0 × 102 to 1.0 × 107 cfu mL-1, with a detection limit of 200 cfu mL-1. Bacteria concentration can be analyzed within 40 min after the sample injection. When applied to test real samples (raw chicken meat) it provided good recoveries (100-111%). An enrichment process was also explored to increase the bacteria concentration, enabling a quantitative detection of Salmonella spp. This biosensor opens a new opportunity for the detection of pathogenic bacteria using bacteriophage.


Assuntos
Carga Bacteriana/métodos , Bacteriófago M13/fisiologia , Técnicas Biossensoriais/métodos , Salmonella/isolamento & purificação , Sequência de Aminoácidos , Animais , Bacteriófago M13/química , Galinhas/microbiologia , Técnicas Eletroquímicas/métodos , Eletrodos , Contaminação de Alimentos/análise , Microbiologia de Alimentos , Ouro/química , Limite de Detecção , Peptídeos/química , Reprodutibilidade dos Testes , Salmonella/química , Ligação Viral
18.
Mikrochim Acta ; 185(2): 148, 2018 02 01.
Artigo em Inglês | MEDLINE | ID: mdl-29594556

RESUMO

A stir foam composed of graphene oxide, poly(ethylene glycol) and natural latex (GO-PEG-NL) was prepared for use in micro-solid phase extraction sorbent of preservative agents and antioxidants from cosmetic products. The extracted analytes were quantified by GC-MS. Under the optimized conditions, the calibration plots are linear in the concentration ranges between 5.0 µg·L-1 to 1.0 mg·L-1 for benzoic acid, of 10.0 µg·L-1 to 1.0 mg·L-1 for 2-methyl-3-isothiazolinone (MI), and between 1.0 µg·L-1 and 1.0 mg·L-1 for both 3-tert-butyl-4-hydroxyanisole (BHA) and 2,6-di-tert-butyl-p-hydroxytoluene (BHT). The LODs are 1.0 µg·L-1 for benzoic acid, 5.0 µg·L-1 for MI and 0.5 µg·L-1 for both BHA and BHT. The stir-foam can be easily prepared, is inexpensive and well reproducible (RSDs <3%, for n = 6). It can be re-used for up to 12 times after which extraction efficiency has dropped to 90%. The method was successfully applied to the determination of preservatives and antioxidants in cosmetic samples. Recoveries from spiked samples ranged between 94.5 ± 2.1% and 99.8 ± 1.8%. Graphical abstract A stir foam was prepared from graphene oxide, poly(ethylene glycol) and natural latex (GO-PEG-NL) and is shown to be a most viable sorbent for the microextraction of trace amounts of preservative agents and antioxidants from cosmetic products.


Assuntos
Antioxidantes/isolamento & purificação , Conservantes Farmacêuticos/isolamento & purificação , Microextração em Fase Sólida/métodos , Hidroxianisol Butilado/análise , Hidroxitolueno Butilado/análise , Cosméticos/análise , Cromatografia Gasosa-Espectrometria de Massas , Grafite/química , Látex/química , Limite de Detecção , Polietilenoglicóis/química
19.
Biosens Bioelectron ; 102: 217-225, 2018 Apr 15.
Artigo em Inglês | MEDLINE | ID: mdl-29149687

RESUMO

A label-free electrochemical miRNA biosensor was developed based on a pyrrolidinyl peptide nucleic acid (acpcPNA)/polypyrrole (PPy)/silver nanofoam (AgNF) modified electrode. The AgNF was electrodeposited as redox indicator on a gold electrode, which was then functionalized with an electropolymerized layer of PPy, a conducting polymer, to immobilize the PNA probes. The fabrication process was investigated by electrochemical impedance spectroscopy. The biosensor was used to detect miRNA-21, a biomarker abnormally expressed in most cancers. The signal was monitored by the change in current of the AgNF redox reaction before and after hybridization using cyclic voltammetry. Two PNA probe lengths were investigated and the longer probe exhibited a better performance. Nucleotide overhangs on the electrode side affected the signal more than overhangs on the solution side due to the greater insulation of the sensing surface. Under optimal conditions, the electrochemical signal was proportional to miRNA-21 concentrations between 0.20fM and 1.0nM, with a very low detection limit of 0.20fM. The biosensor showed a high specificity which could discriminate between complementary, single-, doubled-base mismatched, and non-complementary targets. Three out of the seven tested plasma samples provided detectable concentrations (63 ± 4, 111 ± 4 and 164 ± 7fM). The sensor also showed good recoveries (81-119%). The results indicated the possibilities of this biosensor for analysis without RNA extraction and/or amplification, making the sensor potentially useful for both the prognosis and diagnosis of cancer in clinical application.


Assuntos
Técnicas Biossensoriais , Técnicas Eletroquímicas , MicroRNAs/isolamento & purificação , Hibridização de Ácido Nucleico/genética , Espectroscopia Dielétrica , Ouro/química , Humanos , Limite de Detecção , MicroRNAs/genética , Neoplasias/diagnóstico , Neoplasias/genética , Polímeros/química , Pirróis/química , Pirrolidinas/química , Prata
20.
Anal Chim Acta ; 985: 69-78, 2017 Sep 08.
Artigo em Inglês | MEDLINE | ID: mdl-28864196

RESUMO

Phthalate esters (PAEs), especially dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), di-2-ethylhexyl phthalate (DEHP) are widely used as plasticizers in plastics and polymers. They are not chemically bound and can easily migrate into food and human tissue that comes into contact with these materials. The method developed in this work was applied for the preconcentration and determination of these four phthalate esters that might leach from contact lenses and baby teethers. A novel stir-bead micro-solid phase extractor of chitosan cryogel composited with polypyrrole with a steel wire core was evaluated for the extraction of DMP, DEP, DBP and DEHP before analysis by high performance liquid chromatography (HPLC). Scanning electron micrographs of the polypyrrole-chitosan cryogel beads revealed a high porosity with large surface area. Under the optimum conditions, the developed method provided a good linearity in a concentration range from 10 to 750 ng mL-1 for DMP and from 5.0 to 750 ng mL-1 for DEP, DBP and DEHP. The limits of detection (LOD) were 6.07 ± 0.22 ng mL-1, 4.358 ± 0.097 ng mL-1, 4.408 ± 0.099 ng mL-1 and 3.916 ± 0.053 ng mL-1 for DMP, DEP, DBP and DEHP, respectively, and the method reproducibility was good (n = 6, % RSD < 6.0). DBP and DEHP were detected in two original storage solutions of contact lenses from 13.2 ± 1.1 ng mL-1 to 15.4 ± 1.9 ng mL-1 and from 21.3 ± 1.6 ng mL-1 to 23.5 ± 1.5 ng mL-1, respectively. In the artificial saliva in contact with baby teether samples only DEHP was found, from 4.91 ± 0.31 ng mL-1 to 6.78 ± 0.23 ng mL-1, with good recoveries ranging from 81.3 ± 8.4% to 106.3 ± 5.2%.


Assuntos
Quitosana , Soluções para Lentes de Contato/análise , Criogéis , Ácidos Ftálicos/análise , Polímeros , Pirróis , Saliva Artificial/análise , Ésteres , Reprodutibilidade dos Testes
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