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1.
Appl Opt ; 63(1): 122-128, 2024 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-38175008

RESUMO

This work presents a portable optical meter for noncontact thickness measurement. The device shines a focused laser light on a thin and transparent sample, resulting in an interference between light reflecting from the top and from the bottom surface, and the interfering pattern is recorded by a linear sensor array before data analysis with an Arduino microcontroller. The device produced accurate thickness values from glass cover slips and transparent plastic sheets within a fraction of a second per measurement. Additionally, the sample's refractive index is not required a priori. Therefore, it has a high potential to be of use in real-time quality control in transparent thick-film coating and manufacturing.

2.
Mikrochim Acta ; 190(8): 286, 2023 07 07.
Artigo em Inglês | MEDLINE | ID: mdl-37417989

RESUMO

The application of copper-based nanoparticles synthesized via green synthesis and their integration with a wearable electrode is reported for designing a flexible catalytic electrode on a glove for onsite electroanalysis of paraquat. A copper precursor and an orange extract from Citrus reticulata are used to synthesize an economical electrocatalytic material for supporting the selective and sensitive detection of paraquat. The electrode yields multidimensional fingerprints due to two redox couples in a square wave voltammogram, corresponding to the presence of paraquat. The developed lab-on-a-finger sensor provides the fast electroanalysis of paraquat within 10 s, covering a wide range from 0.50 to 1000 µM, with a low detection limit down to 0.31 µM and high selectivity. It is also possible to use this sensor at a fast scan rate as high as 6 V s-1 (< 0.5 s for a scan). This wearable glove sensor allows the user to directly touch and analyze samples, such as surfaces of vegetables and fruits, to screen the contamination. It is envisioned that these glove-embedded sensors can be applied to the on-site analysis of food contamination and environments.


Assuntos
Nanopartículas , Dispositivos Eletrônicos Vestíveis , Cobre , Paraquat/análise , Eletrodos
3.
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
4.
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
5.
Langmuir ; 37(49): 14302-14313, 2021 12 14.
Artigo em Inglês | MEDLINE | ID: mdl-34859679

RESUMO

Flexible electronics have gained more attention for emerging electronic devices such as sensors, biosensors, and batteries with advantageous properties including being thin, lightweight, flexible, and low-cost. The development of various forms of allotropic carbon papers provided a new dry-manufacturing route for the fabrication of flexible and wearable electronics, while the electrochemical performance and the bending stability are largely influenced by the bulk morphology and the micro-/nanostructured domains of the carbon papers. Here, we evaluate systematically the intrinsic physicoelectrochemical properties of allotropic carbon-based conducting papers as flexible electrodes including carbon-nanotubes-paper (CNTs-paper), graphene-paper (GR-paper), and carbon-fiber-paper (CF-paper), followed by functionalization of the allotropic carbon papers for the fabrication of flexible electrodes. The morphology, chemical structure, and defects originating from the allotropic nanostructured carbon materials were characterized by scanning electron microscopy (SEM) and Raman spectroscopy, followed by evaluating the electrochemical performance of the corresponding flexible electrodes by cyclic voltammetry and electrochemical impedance spectroscopy. The electron-transfer rate constants of the CNTs-paper and GR-paper electrodes were ∼14 times higher compared with the CF-paper electrode. The CNTs-paper and GR-paper electrodes composed of nanostructured carbon showed significantly higher bending stabilities of 5.61 and 4.96 times compared with the CF-paper. The carbon-paper flexible electrodes were further functionalized with an inorganic catalyst, Prussian blue (PB), forming the PB-carbon-paper catalytic electrode and an organic conducting polymer, poly(3,4-ethylenedioxythiophene) (PEDOT), forming the PEDOT-carbon-paper capacitive electrode. The intrinsic attribute of different allotropic carbon electrodes affects the deposition of PB and PEDOT, leading to different electrocatalytic and capacitive performances. These findings are insightful for the future development and fabrication of advanced flexible electronics with allotropic carbon papers.


Assuntos
Grafite , Nanotubos de Carbono , Técnicas Eletroquímicas , Eletrodos , Eletrônica
6.
Mikrochim Acta ; 188(6): 180, 2021 05 05.
Artigo em Inglês | MEDLINE | ID: mdl-33950304

RESUMO

A novel strategy was developed to extract, detect, and quantify trace-level DNA. For the extraction step, a composite of methylene blue (MB), poly(acrylic acid) (PAA), and modified iron oxide magnetic nanoparticles (IOMNPs) (PAA/IOMNPs) was used to adsorb DNA from the sample. MB-PAA/IOMNPs with adsorbed DNA were then separated from the solution with an external magnet and MB-DNA was eluted from PAA/IOMNPs with acetic acid. In the detection step, MB-DNA was adsorbed on the surface of 3-aminopropyltriethoxysilane (APTES)-modified glassy carbon electrode via electrostatic force. DNA was quantified by measuring the oxidation peak of MB at a potential -0.13 V vs. Ag/AgCl using differential pulse voltammetry. Under the optimal experimental conditions, the DNA sensor showed linear ranges from 0.001 to 0.005 pg µL-1, 0.005 to 0.070 pg µL-1, and 0.070 to 0.400 pg µL-1 and a limit of detection of 0.87 fg µL-1. The proposed sensor detected trace DNA in real samples with recoveries that ranged from 80.4 to 90.4%.


Assuntos
Fracionamento Químico/métodos , DNA/análise , Técnicas Eletroquímicas/métodos , Resinas Acrílicas/química , Adsorção , DNA/química , DNA/isolamento & purificação , Técnicas Eletroquímicas/instrumentação , Eletrodos , Humanos , Limite de Detecção , Nanopartículas Magnéticas de Óxido de Ferro/química , Azul de Metileno/química , Mucosa Bucal/química , Propilaminas/química , Reprodutibilidade dos Testes , Silanos/química
7.
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
8.
Mikrochim Acta ; 187(12): 646, 2020 11 09.
Artigo em Inglês | MEDLINE | ID: mdl-33165663

RESUMO

A simple, sensitive, and effective adsorptive stripping voltammetric sensor for the detection of trace-level promethazine was created based on a gold nanoparticle-graphene nanoplatelet-modified glassy carbon electrode (AuNP-GrNP/GCE). AuNP-GrNP nanocomposites were synthesized using an electroless deposition process, and the morphology was characterized using UV-vis spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, and energy-dispersive X-ray spectroscopy. The electrochemical behavior and detection of promethazine at the AuNP-GrNP/GCE were investigated utilizing cyclic voltammetry and adsorptive stripping voltammetry. The AuNP-GrNP/GCE showed outstanding synergistic electrochemical activity for promethazine oxidation, a highly active surface area, great adsorptivity, and outstanding catalytic properties. The electrolyte pH, amount of AuNP-GrNP nanocomposite, preconcentration potential (vs. Ag/AgCl), and time were optimized to obtain a high performance electrochemical sensor. Under optimal conditions, the proposed sensor displayed two linear concentration ranges from 1.0 nmol L-1 to 1.0 µmol L-1 and from 1.0 to 10 µmol L-1. The limits of detection and quantitation were 0.40 and 1.4 nmol L-1, respectively. This sensor displayed high sensitivity, a capability for rapid analysis, and excellent repeatability and reproducibility. The developed sensor was effective and practical for promethazine detection in biological fluids and forensic samples, and the obtained results exhibited excellent agreement with the results obtained using the method described in the British Pharmacopoeia. Graphical abstract.


Assuntos
Eletrodos , Ouro/química , Grafite/química , Nanopartículas Metálicas/química , Prometazina/análise , Detecção do Abuso de Substâncias/métodos , Líquidos Corporais/química , Humanos , Limite de Detecção , Microscopia Eletrônica de Varredura/métodos , Prometazina/normas , Padrões de Referência , Reprodutibilidade dos Testes , Análise Espectral/métodos
9.
Mikrochim Acta ; 187(11): 591, 2020 10 06.
Artigo em Inglês | MEDLINE | ID: mdl-33025245

RESUMO

An electrochemical method has been developed to determine iodide in urine using an electrode modified with silver oxide microparticles-poly acrylic acid/poly vinyl alcohol (Ag2OMPs-PAA/PVA). Silver oxide particles were formed by electrochemical oxidation via cyclic voltammetry. The modified electrode exhibited an excellent response to iodide detection by cathodic stripping voltammetry. The fabrication and operation conditions were optimized in terms of PVA concentration, K2HPO4 concentration, amount of AgMPs-PAA/PVA, number of cycles for oxide formation, electrolyte, applied potential (vs. Ag/AgCl), and time. Under the optimum conditions, iodide determination produced a linear range from 1 to 40 µM. The limit of detection was 0.3 µM. Precision was found to be within 7.4% RSD. The developed method was applied to the determination of iodide in urine samples of pregnant women with satisfying recoveries (86 ± 1 to 108 ± 1%). Graphical abstract.


Assuntos
Iodetos/urina , Gravidez/urina , Resinas Acrílicas/química , Técnicas Eletroquímicas/instrumentação , Técnicas Eletroquímicas/métodos , Eletrodos , Feminino , Humanos , Iodetos/química , Iodo/deficiência , Limite de Detecção , Óxidos/química , Álcool de Polivinil/química , Complicações na Gravidez/diagnóstico por imagem , Complicações na Gravidez/urina , Compostos de Prata/química
10.
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
11.
Opt Lett ; 43(15): 3730-3733, 2018 Aug 01.
Artigo em Inglês | MEDLINE | ID: mdl-30067666

RESUMO

In this Letter, we utilize one-dimensional wavelet analysis to improve the quality of morphology images and velocity profiles of optical coherence tomography simultaneously, by performing analysis on the complex time-frequency plane of raw interferograms, prior to image construction. The results indicate a robust signal improvement that also preserves accuracy for both morphology and velocity information and has been demonstrated on a variety of samples with diverse flow speeds and morphologies.

12.
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
13.
Sensors (Basel) ; 18(10)2018 Oct 19.
Artigo em Inglês | MEDLINE | ID: mdl-30347779

RESUMO

Simple, robust, and low-cost nitrate- and ammonium-selective electrodes were made using substrate prepared from household materials. We explored phosphonium-based ILs and poly (methyl methacrylate)/poly(decyl methacrylate)(MMA-DMA) copolymer as matrix materials alternative to classical PVC-based membranes. IL-based membranes showed suitability only for nitrate-selective electrode exhibiting linear concentration range between 5.0 × 10-6 and 2.5 × 10-3 M with a detection limit of 5.5 × 10-7 M. On the other hand, MMA-DMA-based membranes showed suitability for both ammonium- and nitrate-selective electrodes, and were successfully applied to detect NO3- and NH4⁺ in water and soil samples. The proposed ISEs exhibited near-Nernstian potentiometric responses to NO3- and NH4⁺ with the linear range concentration between 5.0 × 10-5 and 5.0 × 10-2 M (LOD = 11.3 µM) and 5.0 × 10-6 and 1.0 × 10-3 M (LOD = 1.2 µM), respectively. The power of ISEs to detect NO3- and NH4⁺ in water and soils was tested by comparison with traditional, portable colorimetric techniques. Procedures required for analysis by each technique from the perspective of a non-trained person (e.g., farmer) and the convenience of the use on the field are compared and contrasted.

14.
Artigo em Inglês | MEDLINE | ID: mdl-28753095

RESUMO

This paper reports the development of a sensitive, high-throughput colorimetric method for the detection of trace mercuric ions (Hg2+). The method is based on the binding of the analyte to gold nanoparticles (AuNPs) modified with Tween-20. Tween-20 was used as a nonionic stabilizer to allow a good dispersion of AuNPs in solution. When mercuric ions were added to the solution, they replaced the Tween-20 stabilizer on the surface of the AuNPs due to their stronger binding affinity. This caused the NPs to aggregate and the color of the solution to change from red to blue. The quantitative analysis of Hg2+ was achieved by plotting the Red Green Blue (RGB) values of the scanned images of the analyte samples in the AuNP solution against concentrations of Hg2+. Since the reaction was carried out in 96-well plates, ninety-six samples were analyzed simultaneously, reducing the cost and time of analysis. The experimental parameters optimized were the concentrations of Tween-20 and NaCl, the reactants ratio, and the incubation time. Under the optimum conditions, the calibration plot of the assay was linear over an Hg2+ concentration range of 0.10-2.00 mg L-1, and the detection limit was 0.050 mg L-1 (S/N  =  3). The selectivity of the technique was high with no significant colorimetric responses to the presence of 100-fold excesses of other metal ions. Quantification was validated with Hg2+ standard solutions and spiked tap and waste water samples, and the accuracy of the technique was confirmed. The developed technique is simple and cost effective because it requires no complicated instruments, yet the results demonstrate it to be a very powerful technique with the potential to be developed for on-site mercury detection.


Assuntos
Colorimetria/métodos , Ouro/química , Mercúrio/análise , Nanopartículas Metálicas/química , Polissorbatos/química , Poluentes Químicos da Água/análise , Íons , Limite de Detecção
15.
Artigo em Inglês | MEDLINE | ID: mdl-27533342

RESUMO

Two important air pollutants, sulfur dioxide (SO2) and nitrogen dioxide (NO2), were sampled and monitored in the spring season in the biggest industrial area of Bhutan. Field measurements of SO2 and NO2 were performed using standard colorimetric methods, and air samples were collected using an active sampling technique. Sampling sites were selected to cover all the potential catchment areas like settlements, staff quarters, shops and schools. The main objective of this sampling work was to see the distribution of these two pollutants from the source of emission (small scale industries) and to obtain and establish a baseline data. The active sampler was first tested and validated in a laboratory using liquid and gas standards of SO2 and NO2. Good linearity from 0.050 to 1.0 µg mL-1 for SO2 and from 0.010 to 1.0 µg mL-1 for NO2 were obtained (R2 > 0.99) with limits of detection of 30 and 50 ng mL-1 for SO2 and NO2, respectively. Daylong sampling was done at selected sites with a range of distances away from the sources of emission. The ambient concentration of SO2 and NO2 were in the range of 0.45-4.46 and 0.56-5.68 µg m-3, respectively.


Assuntos
Poluentes Atmosféricos/análise , Dióxido de Nitrogênio/análise , Dióxido de Enxofre/análise , Butão , Monitoramento Ambiental , Indústrias , Estações do Ano
16.
Artigo em Inglês | MEDLINE | ID: mdl-27231039

RESUMO

A laboratory-built printed circuit board (PCB) passive sampler used for the monitoring of xylene and styrene in copy print shops was re-validated for detecting benzene, toluene and xylene (BTX) and applied for the sampling of ambient air from Hat Yai city, Songkhla, Thailand, in the month of November 2014. For monitoring, the PCB passive samplers were exposed to target analytes in 16 locations covering high to low exposure areas. After sampling, the samplers were thermally desorbed and the analytes were trapped by multi-walled carbon nanotubes packed into a micro-preconcentrator coupled to a gas chromatograph (GC) equipped with a flame ionization detector. At the optimum GC operating conditions, the linear dynamic ranges for BTX were 0.06-5.6 µg for benzene, 0.07-2.2 µg for toluene and 0.23-2.5 µg for xylene with R(2) > 0.99 with the limits of detection being 6.6, 6.8 and 19 ng for benzene, toluene and xylene, respectively. The concentrations of BTX in the 16 sampling sites were in the range of N.D.-1.3 ± 1.6, 4.50 ± 0.76-49.6 ± 3.7 and 1.00 ± 0.21-39.6 ± 3.1 µg m(-3), respectively. When compared to past studies, there had been an increase in the benzene concentration.


Assuntos
Poluentes Atmosféricos/análise , Benzeno/análise , Monitoramento Ambiental/métodos , Tolueno/análise , Xilenos/análise , Cromatografia Gasosa , Cidades , Nanotubos de Carbono , Tailândia
17.
J Sep Sci ; 38(22): 3921-3927, 2015 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-26347144

RESUMO

A magnetic solid-phase extraction sorbent of polypyrrole/silica/magnetite nanoparticles was successfully synthesized and applied for the extraction and preconcentration of sulfonamides in water samples. The magnetite nanoparticles provided a simple and fast separation method for the analytes in water samples. The silica coating increased the surface area that helped to increase the polypyrrole layer. The polypyrrole-coated silica provided a high extraction efficiency due to the π-π and hydrophobic interactions between the polypyrrole and sulfonamides. Several parameters that affected the extraction efficiencies, i.e. the amount of sorbent, pH of the sample, extraction time, extraction temperature, ionic strength, and desorption conditions were investigated. Under the optimal conditions, the method was linear over the range of 0.30-200 µg/L for sulfadiazine and sulfamerazine, and 1.0-200 µg/L for sulfamethazine and sulfamonomethoxine. The limit of detection was 0.30 µg/L for sulfadiazine and sulfamerazine and 1.0 µg/L for sulfamethazine and sulfamonomethoxine. This simple and rapid method was successfully applied to efficiently extract sulfonamides from water samples. It showed a high extraction efficiency for all tested sulfonamides, and the recoveries were in the range of 86.7-99.7% with relative standard deviations of < 6%.

18.
J Sep Sci ; 38(11): 1951-8, 2015 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-25808354

RESUMO

A new mixed-mode cation-exchange sulfonate composite functionalized with multiwalled carbon nanotubes with polyvinyl alcohol cryogel was fabricated and used for the first time as a solid-phase extraction sorbent for the determination of ß-agonists in animal feeds. Feed samples were extracted with 0.20 M phosphoric acid and methanol (1:4, v/v) using ultrasonication, cleaned-up using the developed sorbent to which the ß-agonists bound then finally eluted with 5.0% ammonia in methanol and analyzed by high-performance liquid chromatography. Various parameters that affected the extraction efficiency were optimized. Under the optimal conditions, the developed sorbent strongly interacted with ß-agonists by cationic exchange and hydrophobic and hydrophilic interactions, that provided a high extraction efficiency in the range of 92.8 ± 3.7-104.4 ± 2.3% over a range of 0.04-2.0 mg/kg for salbutamol and ractopamine, and 0.40-8.0 mg/kg for clenbuterol. The relative standard deviations were less than 6.0%. The developed method was successfully applied for the determination of ß-agonists in various types of animal feed and effectively reduced any matrix interference.


Assuntos
Agonistas Adrenérgicos beta/análise , Ração Animal/análise , Criogéis , Nanotubos de Carbono , Extração em Fase Sólida/métodos , Ácidos Sulfônicos/química , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Microscopia Eletrônica de Varredura , Reprodutibilidade dos Testes
19.
Analyst ; 139(23): 6160-7, 2014 Dec 07.
Artigo em Inglês | MEDLINE | ID: mdl-25306849

RESUMO

A novel highly sensitive and selective molecularly imprinted polymer (MIP) cryogel biosensor for determination of microalbumin in urine samples was fabricated. The MIP gel was prepared based on the graft copolymerization of acrylamide with N,N'-methylenebisacrylamide on chitosan using human serum albumin (HSA) as the template. The sub-zero polymerization allowed the solvent to form ice crystals and left a macroporous cryogel structure when it was thawed. After removing the template, the specific imprinted surface on cryogel pore walls was used to detect HSA via a redox mediator (ferrocene), entrapped in the cryogel, using differential pulse voltammetry (DPV). The electrochemical detection was improved by the presence of graphene that has been composited within the polymer. For determination of albumin, the fabricated MIP cryogel biosensor showed a high sensitivity with a wide linear range of 1.0 × 10(-4) to 1.0 × 10(1) mg L(-1) and a low limit of detection of 5.0 × 10(-5) mg L(-1) (S/N = 3). The sensor also provided a very good reusability, i.e., the sensitivity remained >90% after 9 cycles of binding-rewashing (18 analyses per cycle), while the sensitivity only decreased to 90% after 6 weeks of storage at room temperature. The biosensor also showed a good selectivity, both against bovine serum albumin (BSA) and some common possible interfering compounds normally present in urine (ascorbic acid, uric acid, urea, sodium, chloride, potassium and creatinine). The excellent performance of the biosensor was confirmed by analyzing microalbumin in urine samples, and results were in good agreement with those obtained by the standard immunoturbidimetric method (P > 0.05).


Assuntos
Acrilamida/química , Técnicas Biossensoriais/métodos , Quitosana/química , Compostos Ferrosos/química , Grafite/química , Albumina Sérica/química , Criogéis/química , Humanos , Metalocenos , Microscopia Eletrônica de Varredura
20.
Anal Bioanal Chem ; 406(15): 3763-72, 2014 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-24718436

RESUMO

A novel amperometric uric acid biosensor was fabricated by immobilizing uricase on an electrospun nanocomposite of chitosan-carbon nanotubes nanofiber (Chi-CNTsNF) covering an electrodeposited layer of silver nanoparticles (AgNPs) on a gold electrode (uricase/Chi-CNTsNF/AgNPs/Au). The uric acid response was determined at an optimum applied potential of -0.35 V vs Ag/AgCl in a flow-injection system based on the change of the reduction current for dissolved oxygen during oxidation of uric acid by the immobilized uricase. The response was directly proportional to the uric acid concentration. Under the optimum conditions, the fabricated uric acid biosensor had a very wide linear range, 1.0-400 µmol L(-1), with a very low limit of detection of 1.0 µmol L(-1) (s/n = 3). The operational stability of the uricase/Chi-CNTsNF/AgNPs/Au biosensor (up to 205 injections) was excellent and the storage life was more than six weeks. A low Michaelis-Menten constant of 0.21 mmol L(-1) indicated that the immobilized uricase had high affinity for uric acid. The presence of potential common interfering substances, for example ascorbic acid, glucose, and lactic acid, had negligible effects on the performance of the biosensor. When used for analysis of uric acid in serum samples, the results agreed well with those obtained by use of the standard enzymatic colorimetric method (P > 0.05).


Assuntos
Técnicas Biossensoriais/métodos , Quitosana/química , Enzimas Imobilizadas/análise , Nanopartículas Metálicas/química , Nanotubos de Carbono/química , Urato Oxidase/análise , Ácido Úrico/análise , Ácido Ascórbico/análise , Soluções Tampão , Catálise , Eletroquímica , Eletrodos , Glucose/análise , Concentração de Íons de Hidrogênio , Ácido Láctico/análise , Limite de Detecção , Nanofibras/química , Oxigênio/química , Prata/química , Ácido Úrico/química , Urina/química
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