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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.
J Environ Sci Health B ; 58(4): 334-344, 2023.
Artigo em Inglês | MEDLINE | ID: mdl-36974485

RESUMO

A polypyrrole (PPy)-cotton pad sorbent enclosed in tea bag envelope was developed and used in micro-solid phase extraction (µ-SPE) for the determination of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT). After extraction, the extract was qualified and quantified by a gas chromatograph equipped with a flame ionization detector (GC-FID). Parameters influencing this developed method and the efficiency of µ-SPE were studied and optimized. Under the optimal conditions, the developed method provided good linearity in a concentration range of 0.100-100 µg L-1 for BHA and 0.050-50 µg L-1 for BHT, respectively. The limits of detection were 39.27 ± 0.52 ng L-1 for BHA and 16.96 ± 0.17 ng L-1 for BHT. Satisfactory relative recoveries of BHA and BHT were achieved in the range from 86.8 ± 1.9 to 117.1 ± 2.3% with acceptable relative standard deviation (RSD) below 8.1%. Good reproducibility was obtained with RSDs < 3.1%, for n = 6. The developed adsorbent is easy to operate, low cost, eco-friendly, reusable, with high extraction efficiency, and was successfully applied in the simultaneous synthetic antioxidant determination of non-alcoholic beverage samples.


Assuntos
Antioxidantes , Polímeros , Antioxidantes/análise , Hidroxitolueno Butilado/análise , Pirróis , Hidroxianisol Butilado/análise , Reprodutibilidade dos Testes , Bebidas , Chá
5.
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
6.
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
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 ; 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
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.
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
11.
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
12.
Mikrochim Acta ; 186(12): 822, 2019 11 21.
Artigo em Inglês | MEDLINE | ID: mdl-31754802

RESUMO

A nanosorbent composed of magnetite nanoparticles, graphene oxide and a molecularly imprinted polymer (Fe3O4@SiO2-NH2/GOx/MIP) was synthesized and applied to simultaneous extraction of cephalexin, cefazolin and cefoperazone from milk. The use of magnetite nanoparticles enables fast extraction by using an external magnet. The use of graphene oxide increases extraction affinity, and the MIP improves selectivity. Extraction efficiency was optimized by investigating the effects of the template-to-monomer and cross-linker ratios, the desorption condition, extraction time, salting-out effect, stirring rate, sample volume and amount of adsorbent. The cephalosporins were quantified by using HPLC. Under optimum condition, the linear range of the method extends from 2.5 to 100 µg L-1 for cephalexin and cefazolin, and from 5.0 to 100 µg L-1 for cefoperazone. The limits of detection are 2.5 µg L-1 for cephalexin and cefazolin, and 5 µg L-1 for cefoperazone. The adsorbent was applied to the extraction of cephalosporins from milk, with recoveries in a range from 80.2 to 111.7% and with RSDs of <8.5%. Graphical abstractSchematic representation of a nanocomposite adsorbent consisting of magnetic molecularly imprinted polymer and graphene oxide (GOx). Integrating of magnetite nanoparticles, GOx and high specificity of MIP, the method exhibited a rapid, high extraction efficiency, good selectivity for multi-residue analysis of cephalosporins.


Assuntos
Cefalosporinas/análise , Grafite/química , Nanopartículas de Magnetita/química , Ácidos Polimetacrílicos/química , Adsorção , Animais , Técnicas Biossensoriais , Bovinos , Cromatografia Líquida de Alta Pressão , Limite de Detecção , Fenômenos Magnéticos , Leite/química , Impressão Molecular , Sensibilidade e Especificidade , Dióxido de Silício/química , Extração em Fase Sólida
13.
Mikrochim Acta ; 186(6): 338, 2019 05 09.
Artigo em Inglês | MEDLINE | ID: mdl-31073696

RESUMO

A fluorometric method is described for the detection of ampicillin. A polypyrrole containing fluorescent CdTe quantum dots was incorporated into a silica-based molecularly imprinted polymer. The composite MIP displays good fluorescence (with excitation/emission maxima at 355/548 nm), and high selectivity and affinity for ampicillin due to the use of polypyrrole. Ampicillin is found to quench the fluorescence of composite much more strongly than the emission of a non-imprinted polymer. The imprinting factor of 7.5 implies that the nanocomposite probe contains specific binding sites. The MIP probe has two linear response ranges, one from 0.10 to 25 µg L-1 of ampicillin, and one from 25 to 100 µg L-1. The limit of detection is 0.05 µg L-1. The method was applied to the determination of ampicillin in (spiked) milk and meat samples and gave recoveries between 81.7 and 98.7%. The results agreed well with HPLC techniques. Graphical abstract Schematic presentation of nanocomposite fluorescence probe of polypyrrole and quantum dots incorporated in a molecularly imprinted polymer. Integrating of QDs, high specificity of MIPs and high affinity of polypyrrole, the method exhibited highly sensitive and selective for ampicillin detection.

14.
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.

15.
Anal Bioanal Chem ; 410(27): 7185-7193, 2018 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-30167743

RESUMO

A hierarchically porous structured composite monolith sorbent of polypyrrole-coated graphene oxide and octadecyl silica incorporated in chitosan cryogel (PPY/GOx/C18/chitosan) was synthesized and used as solid-phase extraction sorbent for the determination of carbamate pesticides. Various factors affecting the characteristics of the adsorbents (chemistry of the sorbent, polymerization time, concentrations of graphene oxide and octadecyl silica) and the extraction efficiency using the prepared sorbents, such as sample loading, desorption conditions, sample volume, sample flow rate, sample pH, and ionic strength, were investigated and optimized. Under the optimal conditions of sorbent preparation and extraction, the developed composite monolith sorbent provided wide linear responses from 1.0 to 500 µg L-1 for carbofuran and diethofencarb, from 0.5 to 500 µg L-1 for carbaryl, and from 2.0 to 500 µg L-1 for isoprocarb. The limits of detection using HPLC-UV at 203, 220, and 208 nm were in the range of 0.5-2.0 µg L-1. When the composite monolith sorbent was applied for the pre-concentration and determination of carbamate in fruit juices, good recoveries (84.1-99.5%) were achieved. The developed sorbents were porous and exhibited low back pressure enabling their use at high flow rates during sample loading. Extraction and clean-up were highly efficient, and the good physical and chemical stability of the sorbent enables reuse up to 13 times. Graphical abstract ᅟ.


Assuntos
Carbamatos/isolamento & purificação , Quitosana/química , Criogéis/química , Sucos de Frutas e Vegetais/análise , Grafite/química , Praguicidas/isolamento & purificação , Polímeros/química , Pirróis/química , Adsorção , Carbamatos/análise , Cromatografia Líquida de Alta Pressão/métodos , Análise de Alimentos/métodos , Limite de Detecção , Praguicidas/análise , Porosidade , Reprodutibilidade dos Testes , Extração em Fase Sólida/métodos
16.
J Sep Sci ; 41(20): 3892-3901, 2018 Oct.
Artigo em Inglês | MEDLINE | ID: mdl-30098128

RESUMO

A calix[4]arene-functionalized graphene oxide/polydopamine-coated cellulose acetate adsorbent was fabricated for the pre-concentration of aflatoxins. The highly porous developed adsorbent does not produce the high backpressure that normally occurs in particle-packed cartridges and its large surface area helps to improve adsorption. The highly efficient adsorption of aflatoxins by the hybrid adsorbent is facilitated via hydrogen bonding and hydrophobic and π-π interactions. Polymerization time, amount of calix[4]arene-functionalized graphene oxide, type and volume of desorption solvent, sample pH, sample volume, and sample flow rate were optimized. The linearity of aflatoxin B1 was in the range of 0.01-10.0 µg/kg, aflatoxin B2 was in the range of 0.02-10.0 µg/kg and aflatoxin G1 and aflatoxin G2 were in the range of 0.050-10.0 µg/kg. The limits of detection were 0.01 µg/kg for aflatoxin B1, 0.02 µg/kg for aflatoxin B2 and 0.05 µg/kg for aflatoxin G1 and aflatoxin G2. The developed calix[4]arene-functionalized graphene oxide/polydopamine-coated cellulose acetate adsorbent was successfully utilized for the analysis of aflatoxins from corn samples and the extraction efficiency was satisfactory with obtained recoveries from 83.0 to 106.7%. Moreover, fabricated adsorbent is easy to prepare, inexpensive, and can be reused.


Assuntos
Aflatoxinas/análise , Calixarenos/química , Celulose/análogos & derivados , Indóis/química , Fenóis/química , Polímeros/química , Extração em Fase Sólida , Zea mays/química , Adsorção , Celulose/química , Grafite/química , Concentração de Íons de Hidrogênio , Estrutura Molecular , Óxidos/química , Tamanho da Partícula , Propriedades de Superfície
17.
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
18.
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.

19.
Anal Bioanal Chem ; 409(20): 4697-4707, 2017 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-28685175

RESUMO

A hybrid molecularly imprinted polymer (MIP)-coated quantum dot (QD) nanocomposite was synthesized and applied as a fluorescence probe for the highly sensitive and selective determination of salbutamol. The hybrid MIP-coated QD nanocomposite was synthesized via a copolymerization process in the presence of thioglycolic acid capped CdTe QDs with salbutamol as a template, 3-aminopropyltriethoxysilane as the functional monomer, and tetraethyl orthosilicate as a cross-linker. The optimum molar ratio of template, monomer, and cross-linker was 1:6:20. The fluorescence intensity of the hybrid MIP-coated QDs was efficiently quenched after salbutamol rebound to the recognition sites, as a result of charge transfer from QDs to salbutamol. The synthesized hybrid MIP-coated QD nanocomposite showed high sensitivity and good selectivity toward salbutamol. Under the optimal recognition conditions, the fluorescence intensity was quenched linearly with increasing concentration of salbutamol in the range from 0.10 to 25.0 µg L-1, with a detection limit of 0.034 µg L-1. The hybrid optosensor developed was successfully applied in the determination of salbutamol in animal feeds and meat samples. Satisfactory recoveries were obtained in the range from 85% to 98%, with a standard deviation of less than 8%. Furthermore, the accuracy of the hybrid MIP-coated QD nanocomposite was investigated by comparison with a conventional high-performance liquid chromatography method, with the results obtained with two methods agreeing well with each other. The advantages of this sensing method are simplicity, rapidity, cost-effectiveness, high sensitivity, and good selectivity. Graphical Abstract The synthesis of hybrid MIP-coated QDs nanocomposite.


Assuntos
Agonistas de Receptores Adrenérgicos beta 2/análise , Albuterol/análise , Ração Animal/análise , Carne/análise , Impressão Molecular/métodos , Nanocompostos , Polímeros/química , Pontos Quânticos , Animais , Concentração de Íons de Hidrogênio , Limite de Detecção , Microscopia Eletrônica de Varredura , Reprodutibilidade dos Testes , Espectroscopia de Infravermelho com Transformada de Fourier , Termogravimetria
20.
J Sep Sci ; 39(18): 3602-9, 2016 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-27449825

RESUMO

Magnetite nanoparticles incorporated into alginate beads and coated with a polypyrrole adsorbent were prepared (polypyrrole/Fe3 O4 /alginate bead) and used as an effective magnetic solid-phase extraction sorbent for the extraction and enrichment of endocrine-disrupting compounds (estriol, ß-estradiol and bisphenol A) in water samples. The determination of the extracted endocrine-disrupting compounds was performed using high-performance liquid chromatography with a fluorescence detector. The effect of various parameters on the extraction efficiency of endocrine disrupting compounds were investigated and optimized including the type and amount of sorbent, sample pH, extraction time, stirring speed, and desorption conditions. Under optimum conditions, the calibration curves were linear in the concentration range of 0.5-100.0 µg/L, and the limit of detection was 0.5 µg/L. The developed method showed a high extraction efficiency, the recoveries were in the range of 90.5 ± 4.1 to 98.2 ± 5.5%. The developed sorbent was easy to prepare, was cost-effective, robust, and provided a good reproducibility (RSDs < 5%), and could be reused 16 times. The developed method was successfully applied for the determination of endocrine-disrupting compounds in water samples.


Assuntos
Alginatos/química , Disruptores Endócrinos/isolamento & purificação , Nanopartículas de Magnetita/química , Polímeros/química , Pirróis/química , Extração em Fase Sólida/métodos , Poluentes Químicos da Água/isolamento & purificação , Adsorção , Cromatografia Líquida de Alta Pressão , Disruptores Endócrinos/química , Ácido Glucurônico/química , Ácidos Hexurônicos/química , Limite de Detecção , Extração em Fase Sólida/instrumentação , Poluentes Químicos da Água/química
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