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1.
J Environ Manage ; 300: 113707, 2021 Dec 15.
Artigo em Inglês | MEDLINE | ID: mdl-34534759

RESUMO

Selective removal of contaminants from water by membranes is of practical importance for water purification and environmental protection. In the present study, through an in-situ polymerization process, a novel composite of Fe3O4/molecularly imprinted resorcinol -formaldehyde-melamine resin (Fe3O4/MIRFMR) was synthesized. Then, the novel membrane was prepared from a tea filter bag (TFB) as a base substrate which was subsequently coated by a casting solution containing polyvinylidene fluoride (PVDF) matrix, Prunus scoparia gum as a hydrophilic agent and Fe3O4/MIRFMR as selective filler by phase inversion technique. Resorcinol as functional monomers with multiple hydrophilic groups such as -OH, -NH2 and -NH-, were used for selective removal of Rhodamine B (RhB) as target molecule. The Fe3O4/MIRFMR/PVDF/TFB membranes were characterized by FE-SEM, XRD, FTIR, BET, VSM, water contact angle (WCA) and mechanical analysis. The filtration and adsorption of RhB on the prepared membrane was investigated parameters in a cross-module filtration setup. Casting solution containing 0.01 g of Fe3O4/MIRFMR as optimum value showed good wettability, high water flux (42.5 L/m2 h), flux recovery ratio (88.9%), RhB removal efficiency (95.8%). The selectivity of 4.9, 3.3, 2.1 and 2.5 was found to be for RhB compared to AB, MG, EB, and TB dye. It seems that the fabricated membrane could be an effective and selective option for wastewater containing pollutants. The high removal efficiency, fouling resistance, good wettability and stability of the fabricated membrane are promising for use in practical water filtration, especially for selective removal of dyes.


Assuntos
Corantes , Membranas Artificiais , Fenômenos Magnéticos , Polivinil
2.
Mikrochim Acta ; 186(11): 702, 2019 10 16.
Artigo em Inglês | MEDLINE | ID: mdl-31620918

RESUMO

Water compatible hollow porous molecularly imprinted nanospheres (HP-MINs) have been prepared for specific recognition and extraction of the blood pressure regulating drugs valsartan (VAL) and losartan (LOS). All synthetic steps were performed in aqueous medium and without consumption of organic solvents. The morphology and functionality of the materials were characterized by FT-IR, FE-SEM, and TEM techniques. The adsorption and selectivity experiments demonstrate that the HP-MINs possess a high binding capacity, fast kinetics, excellent water dispersibility and remarkable selectivity for VAL and LOS. The HP-MINs were utilized for dispersive solid phase extraction of VAL and LOS prior to their determination by HPLC-UV. Main variables and their interactions on extraction yield were optimized by multivariate analysis with least amount of experiments. Under optimized conditions, the method has a linear response in the 5-2000 µg L-1 concentration range of both VAL and LOS. The limits of detection are 1.5 µg L-1 for VAL and 1.4 µg L-1 for LOS. Graphical abstract Schematic representation of dispersive solid phase extraction (d-SPE) of valsartan (VAL) and losartan (LOS) from urine sample by hollow porous molecularly imprinted nanospheres (HP-MINs).


Assuntos
Losartan/urina , Nanosferas/química , Dióxido de Silício/química , Valsartana/urina , Adulto , Alumínio/química , Carbono/química , Cromatografia Líquida de Alta Pressão , Feminino , Humanos , Limite de Detecção , Losartan/isolamento & purificação , Masculino , Impressão Molecular , Polimerização , Polímeros/química , Porosidade , Silanos/química , Extração em Fase Sólida/métodos , Valsartana/isolamento & purificação
3.
J Sep Sci ; 38(16): 2797-803, 2015 Aug.
Artigo em Inglês | MEDLINE | ID: mdl-26082081

RESUMO

A molecularly imprinted polymer was selectively applied for solid-phase extraction and diazinon residues enrichment before high-performance liquid chromatography. Diazinon was thermally copolymerized with Fe3 O4 @polyethyleneglycol nanoparticles, methacrylic acid (functional monomer), 2-hydroxyethyl methacrylate (co-monomer), and ethylene glycol dimethacrylate (cross-linking monomer) in the presence of acetonitrile (porogen) and 2,2-azobisisobutyronitrile (initiator). Then, the imprinted diazinon was reproducibly eluted with methanol/acetic acid (9:1, v/v). The sorbent particles were characterized by X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy. The comprehensive study of variables through experimental design showed that the maximum performance was achieved under these conditions: pH 7, 10 mL sample volume, 15 mg sorbent, 10 min vortex time, 5 min ultrasonic time, 200 µL methanol/acetic acid (9:1, v/v) as eluent, and 5 min desorption time. Under optimized conditions, the molecularly imprinted polymer solid-phase extraction method demonstrated a linear range (0.02-5 g/mL), a correlation coefficient of 0.997, and 0.005 g/mL detection limit.


Assuntos
Diazinon/isolamento & purificação , Polímeros/química , Extração em Fase Sólida/métodos , Cromatografia Líquida de Alta Pressão , Diazinon/química , Magnetismo , Impressão Molecular , Polímeros/síntese química , Extração em Fase Sólida/instrumentação
4.
J AOAC Int ; 95(6): 1797-802, 2012.
Artigo em Inglês | MEDLINE | ID: mdl-23451399

RESUMO

A cloud point extraction procedure for the preconcentration of Pb2+ in various samples following complexation with 2,2'-(1E,1'E)-1,1'-(2,2'-azanediylbis(ethane-2,1-diyl)bis(azan-1-yl-1-ylidene)) bis(ethan-1-yl-1-ylidene)diphenol in Triton X-114 after centrifugation is reported. A 0.5 mL portion of methanol acidified with 1.0 M HNO3 was added to the surfactant-rich phase prior to analysis by flame atomic absorption spectrometry. The influence of analytical parameters--including pH, concentrations of ligand, Triton X-114, and HNO3, bath temperature, heating time, and centrifugation rate and time--were optimized, and the effect of the matrix ions on the recovery of Pb2+ was investigated. An LOD of 1.9 ng/mL along with a preconcentration factor of 50 with RSD of 1.0% for Pb2+ were achieved. The proposed procedure was applied to the analysis of various real samples.


Assuntos
Poluentes Ambientais/análise , Análise de Alimentos/métodos , Chumbo/análise , Soluções Tampão , Calibragem , Poluentes Ambientais/química , Concentração de Íons de Hidrogênio , Indicadores e Reagentes , Chumbo/química , Limite de Detecção , Ácido Nítrico/química , Octoxinol , Polietilenoglicóis , Reprodutibilidade dos Testes , Espectrofotometria Atômica , Tensoativos , Temperatura , Nicotiana/química
5.
Carbohydr Polym ; 254: 116806, 2021 Feb 15.
Artigo em Inglês | MEDLINE | ID: mdl-33357837

RESUMO

A reactive and mechano-chemically stable support was prepared from Ag-nanoparticles decorated polyester fabric which was subsequently coated by a casting solution containing polyvinylidene fluoride matrix, guar gum (GG) exo-polysaccharide hydrophilic agent, and UiO-66 filler. FE-SEM, XRD, FT-IR, water contact angle technique, and mechanical stability tests were applied to characterize the prepared membranes. The water contact angle measurements indicated the hydrophilicity of the prepared membrane which can be attributed to the nature of bio-GG and UiO-66. The prepared membrane was employed for purifying contaminated waters containing N-cetyl-N,N,N-trimethylammonium bromide (CTAB) and congo-red (CR) dye through a cross-module set-up. The central composite design was also exploited to study the effect of operational parameters such as CTAB and CR concentration, pH solution, and pressure on the removal efficiency. Particularly, the bio-based GG/UiO-66 dispersion showed excellent self-healing properties, which enabled an effective pollutant separation ability and facilitated the recyclability/sustainability of the as-prepared membrane.


Assuntos
Galactanos/química , Mananas/química , Gomas Vegetais/química , Poliésteres/química , Purificação da Água/métodos , Cetrimônio/isolamento & purificação , Corantes/isolamento & purificação , Vermelho Congo/isolamento & purificação , Interações Hidrofóbicas e Hidrofílicas , Membranas Artificiais , Nanopartículas Metálicas/ultraestrutura , Microscopia de Força Atômica , Microscopia Eletrônica de Varredura , Estrutura Molecular , Polivinil , Prata , Espectroscopia de Infravermelho com Transformada de Fourier , Têxteis , Poluentes Químicos da Água/isolamento & purificação , Difração de Raios X
6.
Talanta ; 232: 122449, 2021 Sep 01.
Artigo em Inglês | MEDLINE | ID: mdl-34074433

RESUMO

Antibiotics, such as sulfadiazine and sulfathiazole, are widely used in veterinary applications which can result in remains in edible animal products. Therefore, there is an immense need for a reliable, selective, sensitive, and simple analytical technique for monitoring the concentration of sulfadiazine (SDZ) and sulfathiazole (STZ) in edible animal products. In this regard, we developed a magnetic dual template molecularly imprinted polymer (MMIP) to determine the SDZ and STZ in milk samples. For the sensitive and selective extraction and determination of target analytes, MMIPs have been combined with the syringe-to-syringe magnetic solid-phase microextraction (SS-MSPME) method. In addition, we used central composite design (CCD) for the extraction of SDZ and STZ. With optimum conditions, an efficient, rapid, and convenient technique for the preconcentration and determination of SDZ and STZ in milk samples by SS-MSPME coupling with HPLC-UV was developed. Using our combined approach, the limits of detection are 0.9 and 1.3 ng mL-1 for SDZ and STZ, respectively, along with good linearity and determination coefficients higher than 0.98. Our method demonstrates a practical approach for the deduction of antibiotics in milk samples with high recoveries and selectivity.


Assuntos
Impressão Molecular , Sulfadiazina , Animais , Cromatografia Líquida de Alta Pressão , Fenômenos Magnéticos , Leite/química , Polímeros Molecularmente Impressos , Extração em Fase Sólida , Sulfadiazina/análise , Sulfatiazóis , Seringas
7.
Talanta ; 221: 121620, 2021 Jan 01.
Artigo em Inglês | MEDLINE | ID: mdl-33076148

RESUMO

In this study, a magnetic molecularly imprinted polymer (MMIP (Fe3O4@SiO2-MIP)) was used for the dispersive magnetic solid-phase microextraction (d-MSP-µ-E) to design an easy and effective method for melatonin (MLT) extraction in the methanolic extract of Portulaca oleracea, human urine and plasma, and water samples. HPLC with UV detection was utilized, and pH, the type and volume of eluent, MMIP mass, and contact time were considered as effective factors in the study of MLT separation and pre-concentration. These factors were optimized by Plackett-Burman and multi-objective response surface methodology (RSM). The values were 10 mg, 14 min, 4.2, methanol, 0.180 mL, 2.5 min, for the MMIP mass, time of sorption, sample pH, eluent type, eluent volume, and time of elution, respectively. At the optimum conditions, the limit of detection (LOD) was 0.046 ng mL-1, and the limit of quantification (LOQ) was 0.156 ng mL-1. The sorption capacity of the proposed MMIP sorbent was 109.1 mg g-1 at the optimum conditions. Besides, linear dynamic range (LDR) was 0.2-4200 ng mL-1, and the precision of the method (RSD %) for triplicate measurements was <6.1%. The MMIP showed saturation magnetization of 19.75 emu g-1, resulting in fast separation of the sorbent. The sorption test revealed the high sorption capacity of the MMIP for MLT and its homogeneous binding sites. In all spiked levels (50, 100, 200, and 500 ng mL-1), 93.07-104.1% was the range obtained for the recovery of MLT. The relative selectivity factor (ß) values of MLT/tryptophan, MLT/serotonin, MLT/ferulic acid, MLT/mefenamic acid, MLT/quercetin, MLT/luteolin, and MLT/chlorogenic acid were 1.60, 1.68, 2.02, 2.38, 2.32, 2.40, and 2.50, respectively. The results of desorption-regeneration cycles (seven times) by employing the MMIP showed the high stability of the resultant material. In conclusion, the MMIP combined with the magnetic separation showed a specific sorption behavior for MLT and suggested a simple, flexible, selective, and powerful analytical tool.


Assuntos
Melatonina , Impressão Molecular , Portulaca , Adsorção , Cromatografia Líquida de Alta Pressão , Humanos , Limite de Detecção , Metanol , Extratos Vegetais , Polímeros , Dióxido de Silício , Água
8.
Biosens Bioelectron ; 165: 112346, 2020 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-32729487

RESUMO

A simple and highly sensitive photoelectrochemical biosensor towards L-phenylalanine, as a kind of typical essential amino acid and phenylketonuria biomarker was developed on a surface molecular imprinted (MIP) polydopamine-coated CdS/CdSe/Zn heterojunction. Hierarchical marigold flower-like Zn layer decorated by n-type dichalcogenides interfacial heterojunction was successfully designed and synthesized on Ti foil for PEC converter by in situ electrodeposition. A visible-light-driven molecular imprinting film was prepared through the electropolymerization of dopamine in the presence of L-Phe as biomarker. The combination of bio-MIP and photoelectrochemistry overcomes the defects of the PEC method, which is the absence of selectivity, and offers a new PEC sensor with high sensitivity and selectivity based on visible-light-driven heterojunction and biopolymer-enhanced strategy. The unique interfacial between the Zn marigold flower layer as low work function support and CdS/CdSe n-n heterojunction as well as n-type characteristics of polydopamine imprinted by L-Phe biomarker drastically increase the light trapping and absorption in the visible range, and dramatically inhibit the charge carrier recombination, which is crucial for boosting the Bio-PEC activity. Photocatalytic, electrocatalytic and physicochemical properties of the above-mentioned layers were fully characterized. As-prepared PEC biosensor displayed superb performance for the detection of L-Phe biomarker in the optimized condition obtained from central composite design modeling, showing two linear range 0.005-2.5 and 2.5-130 µM and a low detection limit of 0.9 nM. This work suggests that such L-Phe-imprinted polydopamine-coated Zn/CdS/CdSe heterojunction is greatly promising for being applied in photoelectrochemical biosensing with high photo-electron conversion efficiency.


Assuntos
Técnicas Biossensoriais , Compostos de Cádmio , Fenilcetonúrias , Compostos de Selênio , Técnicas Eletroquímicas , Humanos , Indóis , Limite de Detecção , Fenilalanina , Fenilcetonúrias/diagnóstico , Polímeros
9.
Chemosphere ; 259: 127440, 2020 Nov.
Artigo em Inglês | MEDLINE | ID: mdl-32590178

RESUMO

A new mixed matrix membrane (MMM) was prepared by incorporating biological mesoporous carbon microspheres (mCMSs) from corn starch polysaccharide-supported hydrophilic polydopamine (PDA), as a mesoporous and large-surface area filler, selective modifier, and pore-forming agent, into polyvinylidene fluoride (PVDF) matrix in presence of polyethylene glycol (PEG) as a hydrophilic agent. The structural parameters of the prepared membranes were characterized via FE-SEM, BET/BJH, XRD, FT-IR, and AFM analyses, sorption experiments, water permeability assessments, porosimetry tests, flux recovery ratio (FRR) evaluations, and contact angle measurements, with the so-called central composite design (CCD) been successfully applied for optimization and investigation of the effects of the operational parameters. The results were then applied to treat double-distilled water containing bovine serum albumin (BSA) utilizing a cross-module set-up. Based on the findings, the content of the mCMS-PDA in the PVDF matrix significantly affected the contact angle, pure water flux (PWF), FRR, and BSA removal. In this respect, the PWF of the PVDF-PEG-mCMS-PDA increased from 10.25 to 27.78 L/m2 h with increasing the mCMS-PDA content, with the peak FRR (93.84%) of the PVDF-PEG-mCMS-PDA seen at maximum surface hydrophilicity of the membrane.


Assuntos
Carbono/química , Membranas Artificiais , Soroalbumina Bovina/química , Purificação da Água/métodos , Interações Hidrofóbicas e Hidrofílicas , Indóis , Microesferas , Permeabilidade , Polímeros , Polivinil , Espectroscopia de Infravermelho com Transformada de Fourier , Água/química , Zea mays
10.
Spectrochim Acta A Mol Biomol Spectrosc ; 226: 117606, 2020 Feb 05.
Artigo em Inglês | MEDLINE | ID: mdl-31614272

RESUMO

Citrate and polyvinyl alcohol capped gold nanoparticles (PVA-GNPs) were synthesized via chemical reduction technique and fully characterized by DLS, SEM, EDS, XRD, UV-Vis and FT-IR analysis. A simple and practical colorimetric sensor based on red-ox reaction of p-dimethylaminobenzaldehyde (DABA) as ehrlich's bio-reagent and Au(III) with H2O2 on PVA-GNPs mimic catalyst with enzyme-like activity, has been fabricated for determination of F-, Br- and I- halide anions. Prepared PVA-GNPs, can simultaneously catalyze the disintegration of H2O2, that used to reduce Au(III) ions into co-doped Au-NPs and oxidation of p-dimethylaminobenzaldehyde ehrlich's bio-reagent while in the presence of halide ions Au-X complex can be formed and improved sensor selectivity. Halide ions (F-, Br- and I-) effectively diminishes the catalytic activity of GNPs to disintegrate oxygenated water by the interaction among Au+ and Au0 and suppressing oxidation of p-dimethylaminobenzaldehyde ehrlich's bio-reagent. In this system which contains PVA-GNPs, H2O2, p-dimethylaminobenzaldehyde ehrlich's bio-reagent, and Au(III), increasing the halide ions (F-, Br- and I-) concentration show color changes from deep green to red. In view of this rule, in this work, a novel colorimetric technique for sensitive determination of F-, Br- and I- was developed. This method has the detection limits of 2.60 × 10-6 M, 6.64 × 10-8 M and 9.93 × 10-9 M and linear ranges between 1.98 × 10-5-1.22 × 10-3 M, 1.99 × 10-6-2.0 × 10-4 M and 1.07 × 10-7- 2.86 × 10-5 M for F-, Br- and I-, respectively. Assays are highly selective over other ions. They effectively applied to detection of halide ions in real water samples.


Assuntos
Benzaldeídos/química , Técnicas Biossensoriais/métodos , Bromo/análise , Flúor/análise , Ouro/química , Iodo/análise , Nanopartículas Metálicas/química , Catálise , Ácido Cítrico/química , Colorimetria/métodos , Íons/análise , Limite de Detecção , Análise Multivariada , Oxirredução , Peroxidases/análise , Peroxidases/metabolismo , Álcool de Polivinil/química
11.
Mater Sci Eng C Mater Biol Appl ; 114: 111023, 2020 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-32994021

RESUMO

Hydrogel membranes (HMs) are defined and applied as hydrated porous media constructed of hydrophilic polymers for a broad range of applications. Fascinating physiochemical properties, unique porous architecture, water-swollen features, biocompatibility, and special water content dependent transport phenomena in semi-permeable HMs make them appealing constructs for various applications from wastewater treatment to biomedical fields. Water absorption, mechanical properties, and viscoelastic features of three-dimensional (3D) HM networks evoke the extracellular matrix (ECM). On the other hand, the porous structure with controlled/uniform pore-size distribution, permeability/selectivity features, and structural/chemical tunability of HMs recall membrane separation processes such as desalination, wastewater treatment, and gas separation. Furthermore, supreme physiochemical stability and high ion conductivity make them promising to be utilised in the structure of accumulators such as batteries and supercapacitors. In this review, after summarising the general concepts and production processes for HMs, a comprehensive overview of their applications in medicine, environmental engineering, sensing usage, and energy storage/conservation is well-featured. The present review concludes with existing restrictions, possible potentials, and future directions of HMs.


Assuntos
Matriz Extracelular , Hidrogéis , Condutividade Elétrica , Polímeros , Porosidade
12.
J AOAC Int ; 92(4): 1208-18, 2009.
Artigo em Inglês | MEDLINE | ID: mdl-19714992

RESUMO

New iodide ion-selective electrodes based on bis(2-methyl-3-phenyl-propenylidene)1,2-propanediamine)mercury(II) bromide [Hg(BMPPMB)Br2], bis (5-bromo salicylaldehyde) ethylenediimine vanadyl(IV) [VO(5-Br Salen)], and bis(5-bromo salicylaldehyde) ethylenediimine uranyl(VI) [UO2(5-Br Salen)] carriers are described. The electrodes exhibited Nernstian slopes of -58.3 +/- 1.0, -58.5 +/- 1.4, and -59.0 +/- 1.2 mV/decade for Hg(BMPPMB)Br2, VO(5-Br Salen), and UO2(5-Br Salen) iodide ion concentration in the range of 1.0 x 10(-6)-0.1 M, with detection limits of about 0.6, 0.5, and 0.3 microM, respectively. The potentiometric responses of the electrodes were independent of pH over the range 1.7-10.6, 2.2-11.3, and 2.1-11.1, with satisfactory reproducibility. The electrodes had response times of < or =5 s and could be used for at least 84, 80, and 100 days for Hg(BMPPMB)Br2, VO(5-Br Salen), and UO2(5-Br Salen), respectively, without any considerable divergence in their potential responses.


Assuntos
Iodetos/análise , Ionóforos/análise , Eletrodos , Grafite , Concentração de Íons de Hidrogênio , Indicadores e Reagentes , Membranas Artificiais , Preparações Farmacêuticas/análise , Cloreto de Polivinila , Potenciometria , Espectrofotometria Ultravioleta
13.
J AOAC Int ; 92(3): 907-13, 2009.
Artigo em Inglês | MEDLINE | ID: mdl-19610384

RESUMO

A cloud point extraction (CPE) procedure was presented for the preconcentration of silver, zinc, and lead ions in various samples. The complexes of these metal ions with 2-(((1H-benzo[d]imidazol-2-yl)methoxy)methyl)-1H-benzo[d]imidazole (BIMMBI) are quantitatively extracted into the Triton X-114-rich phase after centrifugation. A solution of 1.0 M HNO3 in methanol was added to the surfactant-rich phase as the effective eluant before analysis by flame atomic absorption spectrometry. The influence of effective parameters such as the concentrations of BIMMBI, Triton X-114, and HNO3, pH, bath temperature, centrifuge rate, and time on method sensitivity and efficiency was optimized. Detection limits of 2.8, 1.7, and 1.1 ng/mL for Pb2+, Ag+, and Zn2+, respectively, along with a preconcentration factor of 30 and enrichment factors of 33, 48, and 53 for Pb2+, Ag+, and Zn2+, respectively, were obtained. The present CPE method is suitable for accurate and precise determination of trace amounts of analyte ions in complex matrixes. The proposed CPE procedure was applied to the determination of these ions in biological, natural water, wastewater, soil, and blood samples.


Assuntos
Chumbo/análise , Prata/análise , Espectrofotometria Atômica/métodos , Zinco/análise , Concentração de Íons de Hidrogênio , Octoxinol , Polietilenoglicóis/química , Cloreto de Sódio/química , Temperatura , Viscosidade
14.
Int J Biol Macromol ; 139: 40-48, 2019 Oct 15.
Artigo em Inglês | MEDLINE | ID: mdl-31369780

RESUMO

The purpose work is devoted to design of a simple, one-pot and green approach for the synthesis of molecularly imprinted polymer to construct a selective sorbent for pipette-tip solid phase extraction of Rhodamine B from chili powder samples and its subsequence separation and quantification by high performance liquid chromatography-ultraviolet/visible detection. The prepared molecularly imprinted polymer was synthesized using chitosan as versatile natural multi-functional bio-monomer and Rhodamine B as template in aqueous media. The effects of influential parameters (sorbent dosage, flow rate and eluent solvent volume) and their influences on Rhodamine B extraction recovery were examined and optimized by central composite design based response surface methodology as a powerful multivariate optimization tool. Under the optimized conditions, the linear range and limit of detection and quantification of proposed method were achieved to be 0.005-15 mg kg-1, 0.0015 mg kg-1 and 0.00488 mg kg-1, respectively, with satisfactory recoveries (>85.0%) and excellent repeatability (relative standard deviation < 6.1%). The easy synthesis conditions as well as satisfactory figures of merit are good indication of applicability of suggested method for extraction and determination of Rhodamine B from chili powder samples in terms of simplicity, cost effectiveness, selectivity and accurate analysis.


Assuntos
Capsicum/química , Impressão Molecular , Polímeros/síntese química , Rodaminas/isolamento & purificação , Extração em Fase Sólida/métodos , Técnicas de Química Sintética , Custos e Análise de Custo , Química Verde , Polímeros/química , Pós , Extração em Fase Sólida/economia
15.
Biosens Bioelectron ; 132: 105-114, 2019 May 01.
Artigo em Inglês | MEDLINE | ID: mdl-30856426

RESUMO

An ultrasensitive Visible light-triggered photoelectrochemical (PEC) sensor was designed based on ideal photoactive lead sulfoiodide (Pb5S2I6) as low band gap crystal, which hydrothermally synthesized rapidly at low temperature (160 °C) in hydrochloride acid media followed by its incorporation into polydopamine as reactive photo-biointerface, through a facile in situ electropolymerization method, coated on nanoporous TiO2 grown by anodization on Ti foil. The structure of as-prepared samples and their photoelectrochemical properties were fully characterized. This unique photo-sensitive Pb5S2I6 catalyst-based PEC bioassay was constructed for the detection of low-abundant Cr(VI) ion in real samples. Applying central composite design, individual and mutual interaction effects were evaluated to obtain optimized solution pH, applied potential and radiant light wavelength as operational factors influencing the PEC efficiency for Cr(VI) detection. At optimal condition, the proposed sensor due to effective suppress in electron-hole recombinations showed a very low detection limit of 3.0 nM, over a broad linear concentration range of 0.01-80 µM in addition to high sensitivity versus 1.9 µA/µM Cr(VI). Proposed PEC sensor displayed high selectivity, reproducibility and stability as well as improved excitation conversion efficiency, which make it highly applicable using solar energy. The potential applicability of the designed sensor was evaluated in water, tomato juice and hair color.


Assuntos
Técnicas Biossensoriais/métodos , Cromo/análise , Indóis/química , Chumbo/química , Polímeros/química , Titânio/química , Poluentes Químicos da Água/análise , Cristalização , Técnicas Eletroquímicas/métodos , Sucos de Frutas e Vegetais/análise , Iodo/química , Luz , Limite de Detecção , Solanum lycopersicum/química , Nanoporos/ultraestrutura , Processos Fotoquímicos , Porosidade , Reprodutibilidade dos Testes , Enxofre/química , Águas Residuárias/análise
16.
Int J Nanomedicine ; 14: 1669-1685, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-30880972

RESUMO

PURPOSE: Nanoporous membranes have been employing more than before in applications such as biomedical due to nanometer hexagonal pores array. Biofouling is one of the important problems in these applications that used nanoporous membranes and are in close contact with microorganisms. Surface modification of the membrane is one way to prevent biofilm formation; therefore, the membrane made in this work is modified with carbon nanotubes. METHODS: In this work, nanoporous solid-state membrane (NSSM) was made by a two-step anodization method, and then modified with carbon nanotubes (NSSM-multi-wall carbon nanotubes [MWCNT]) by a simple chemical reaction. Techniques such as atomic force microscopy (AFM), energy dispersive X-ray (EDAX), field emission scanning electron microscopy (FESEM), Fourier-transform infrared spectroscopy (FTIR), contact angle (CA), surface free energy (SFE), protein adsorption, flow cytometry, and MTT assay were used for membrane characterization. RESULTS: The BSA protein adsorption capacity reduced from 992.54 to 97.24 (µg mL-1 cm-2) after modification. The findings of flow cytometry and MTT assay confirmed that the number of dead bacteria was higher on the NSSM-MWCNT surface than that of control. Adsorption models of Freundlich and Langmuir and kinetics models were studied to understand the governing mechanism by which bacteria migrate to the membrane surface. CONCLUSION: The cell viability of absorbed bacteria on the NSSM-MWCNT was disrupted in direct physical contact with carbon nanotubes. Then, the dead bacteria were desorbed from the surface of the hydrophilic membrane. The results of this research showed that NSSM-MWCNT containing carbon nanotubes have significant antimicrobial and self-cleaning property that can be used in many biomedical devices without facing the eminent problem of biofouling.


Assuntos
Incrustação Biológica , Membranas Artificiais , Nanoporos , Nanotubos de Carbono/química , Adsorção , Aderência Bacteriana , Escherichia coli/fisiologia , Escherichia coli/ultraestrutura , Cinética , Viabilidade Microbiana , Microscopia de Força Atômica , Espectrometria por Raios X , Espectroscopia de Infravermelho com Transformada de Fourier , Staphylococcus aureus/fisiologia , Staphylococcus aureus/ultraestrutura , Termodinâmica , Água/química
17.
J Chromatogr A ; 1594: 13-22, 2019 Jun 07.
Artigo em Inglês | MEDLINE | ID: mdl-30765129

RESUMO

This paper reports a new variant of sample clean-up procedure based on miniaturized matrix solid phase dispersion (MSPD) combining with water compatible magnetic molecularly imprinted polymers (MMIP) for preconcentration of melamine from milk samples prior high-performance liquid chromatography with UV detection. By employing MMIP as dispersant sorbent matrix interferences could be eliminated completely and the column packing step was interestingly omitted that decreasing in glassware expenditure, labor effort and extraction time which cause improvement of the method performance. In order to investigate the functionality, morphology and magnetic properties of the prepared MMIP, it was fully characterized by FT-IR, VSM, SEM, and TEM. Multivariate optimization was applied as a versatile statistical approach for evaluating the influence of the main variables and their interactions on extraction efficiency. Under optimized conditions, the proposed method exhibited a wide linear response in the concentration range of 250.0-5000.0 µg L-1, satisfactory recoveries for all samples (86.6% ≤), and supreme repeatability (RSD less than 6.3%) were achieved as well. The low limit of detection close to 67.0 µg L-1 implied high ability of proposed method for isolation of melamine from complicate milk sample. These befitting results demonstrated that the developed method is unique in terms of the facility, rapidly and least solvent consumption as well as accurate analysis of melamine at trace levels.


Assuntos
Análise de Alimentos/métodos , Magnetismo , Leite/química , Polímeros/química , Extração em Fase Sólida , Triazinas/isolamento & purificação , Animais , Cromatografia Líquida de Alta Pressão , Impressão Molecular , Solventes/química , Espectroscopia de Infravermelho com Transformada de Fourier , Água/química
18.
Int J Nanomedicine ; 14: 1907-1918, 2019.
Artigo em Inglês | MEDLINE | ID: mdl-30936693

RESUMO

PURPOSE: Alumina substrates are one of the commonly used scaffolds applied in cell culture, but in order to prevent formation of biofilm on the alumina substrate, these substrates are modified with carbon nanotube. METHODS: The alumina substrate was made by a two-step anodization method and was then modified with carbon nanotubes by simple chemical reaction. The substrates were characterized with FTIR, SEM, EDX, 3D laser scanning digital microscope, contact angle (CA) and surface free energy (SFE). To determine how this modification influences the reduction of biofilm, biofilm of two various bacteria, Escherichia coli (E.coli) and Staphylococcus aureus (S. aureus), were investigated. RESULTS: The biofilm on the modified substrate decreased due to the presence of carbon nanotubes and increased antibacterial properties. Dental pulp stem cells (DPSCs) were cultured onto flat alumina (FA) and nanoporous alumina-multiwalled carbon nanotubes (NAMC) substrates to examine how the chemical modification and surface topography affects growth of DPSCs. CONCLUSION: Cell attachment and proliferation were investigated with SEM and Presto Blue assay, and the findings show that the NAMC substrates are suitable for cell culture.


Assuntos
Técnicas de Cultura de Células/instrumentação , Técnicas de Cultura de Células/métodos , Polpa Dentária/citologia , Nanotubos de Carbono , Células-Tronco/citologia , Óxido de Alumínio , Aderência Bacteriana , Biofilmes , Proliferação de Células , Células Cultivadas , Escherichia coli/fisiologia , Humanos , Microscopia Confocal , Microscopia Eletrônica de Varredura , Nanoporos , Espectroscopia de Infravermelho com Transformada de Fourier , Staphylococcus aureus/fisiologia
19.
Talanta ; 195: 390-400, 2019 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-30625559

RESUMO

In this work, novel dummy molecularly imprinted polymers (DMIP) with propanamide as a dummy template molecule were prepared based on a green synthesis strategy of less consumption of hazardous/organic reagents and at mild conditions for magnetic solid-phase extraction (MSPE) of acrylamide in biscuit samples, followed by high performance liquid chromatography (HPLC) determination. The resultant DMIP was well characterized by FT-IR, SEM, TEM and VSM, exhibiting uniform nanoscale coreshell structure and good magnetic property in favor of simple rapid separation. Several main variables influencing MSPE efficiency were investigated, including DMIP dosage, sample solution pH, extraction time and desorption solvent; central composite design (CCD) and response surface methodology (RSM) were employed to assist in the MSPE condition optimization with rapidity and reliability. Under optimized conditions, excellent linearity for acrylamide was obtained in the range of 5.0-5000.0 µg kg-1, and low detection and quantification limits were 1.3 µg kg-1 and 4.4 µg kg-1, respectively. The method recoveries at five spiked concentrations were found within 86.0-98.3% with relative standard deviations (RSDs) of 1.2-4.1%. Furthermore, endogenous acrylamide was detected in five different biscuit samples and the RSDs values were lower than 3.3%. The present study suggested promising perspectives of water-compatible eco-friendly DMIP based MSPE-HPLC method for highly effective sample pretreatment and targeted analytes determination in complicated matrices.


Assuntos
Acrilamida/química , Contaminação de Alimentos/análise , Polímeros/química , Cromatografia Líquida de Alta Pressão/métodos , Química Verde , Impressão Molecular , Extração em Fase Sólida/métodos
20.
J Hazard Mater ; 158(1): 131-6, 2008 Oct 01.
Artigo em Inglês | MEDLINE | ID: mdl-18314265

RESUMO

A new and efficient solid phase extraction method is described for the preconcentration of trace heavy metal ions. The method is based on the adsorption of Fe(3+), Cu(2+) and Zn(2+) on 2-phenyl-1H-benzo[d] imidazole (PHBI) loaded on Triton X-100-coated polyvinyl chloride (PVC). The influences of the analytical parameters including pH and sample volume were investigated. Common coexisting ions did not interfere on the separation and determination of analytes under study. The adsorbed analytes were desorbed by using 5 mL of 4 mol L(-1) nitric acid. The preconcentration factor is 90. The detection limits (3 sigma) were in the range of 0.95-1 microg L(-1). The sorbent exhibited excellent stability and its sorption capacity under optimum conditions has been found to be more than 2.7 mg of ions per gram of sorbent. The recoveries of analytes were generally higher than 95%. The relative standard deviations (R.S.D.s) were generally lower than 4%. The method has been successfully applied to some real samples.


Assuntos
Benzimidazóis/química , Metais Pesados/química , Octoxinol/química , Cloreto de Polivinila/química , Extração em Fase Sólida/métodos , Reutilização de Equipamento , Concentração de Íons de Hidrogênio , Íons/química , Reprodutibilidade dos Testes , Tensoativos/química
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