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1.
J Chromatogr A ; 1717: 464668, 2024 Feb 22.
Artigo em Inglês | MEDLINE | ID: mdl-38278132

RESUMO

An efficient magneto-adsorbent composed of polyaniline blend poly(amidoamine) dendrimers modified graphene oxide quantum dots and magnetic Fe3O4 particles (Fe3O4@PANI-PSS/PAMAM-QGO) for magnetic solid-phase extraction (MSPE) of polycyclic aromatic hydrocarbons (PAHs) in environmental water was synthesized. Fe3O4@PANI-PSS/PAMAM-QGO exhibited exceptional adsorption property for most PAHs analytes. The nanocomposite sorbent demonstrated a ferromagnetic behavior of 17.457 emu g-1, which is adequate for subsequent use in MSPE. Key parameters affecting the processes of adsorption and desorption, including the sorbent amount, vortex adsorption time, vortex extraction time, sample volume, a solvent for desorption and the solvent volume were all examined and optimized. The performance of MSPE using Fe3O4@PANI-PSS/PAMAM-QGO as adsorbent for four PAHs, including fluoranthene, acenaphthene, phenanthrene and pyrene were studied through high performance liquid chromatography equipped with spectrofluorometer. Under the optimal conditions, Fe3O4@PANI-PSS/PAMAM-QGO showed a wide linearity of 10-1,000 ng mL-1, low detection limit (LOD) ranging from 1.92 to 4.25 ng mL -1 and high accuracy (recoveries of 93.6-96.5 %). Enrichment factors up to 185 were achieved. Furthermore, Fe3O4@PANI-PSS/PAMAM-QGO exhibited good recyclability (10 times, RSDs ≤ 5.35%), while maintaining its high efficiency in the extraction of PAHs. The proposed method was successfully applied for environmental samples. Recoveries ranging from 81.2 to 106.2 % were obtained, indicating a low matrix effect and the robustness of the optimized MSPE method. Based on these features and under the optimal extraction conditions, Fe3O4@PANI-PSS/PAMAM-QGO was demonstrated to be a successful tool for the rapid and sensitive extraction of PAHs in the samples.


Assuntos
Compostos de Anilina , Dendrímeros , Grafite , Poliaminas , Hidrocarbonetos Policíclicos Aromáticos , Pontos Quânticos , Poluentes Químicos da Água , Hidrocarbonetos Policíclicos Aromáticos/análise , Água , Adsorção , Pontos Quânticos/análise , Solventes/análise , Fenômenos Magnéticos , Extração em Fase Sólida/métodos , Limite de Detecção , Poluentes Químicos da Água/análise
2.
Sensors (Basel) ; 23(12)2023 Jun 08.
Artigo em Inglês | MEDLINE | ID: mdl-37420598

RESUMO

A simple and rapid method for determining mercury (II) has been developed using L-cysteine-capped copper nanocluster (CuNCs) with o-phenylenediamine (OPD) as the sensor. The characteristic fluorescence peak of the synthesized CuNCs was observed at 460 nm. The fluorescence properties of CuNCs were strongly influenced by the addition of mercury (II). Upon addition, CuNCs were oxidized to form Cu2+. Then, the OPD were rapidly oxidized by Cu2+ to form o-phenylenediamine oxide (oxOPD), as evidenced by the strong fluorescence peak at 547 nm, resulting in a decrease in the fluorescence intensity at 460 nm and an increase in the fluorescence intensity at 547 nm. Under optimal conditions, a calibration curve between the fluorescence ratio (I547/I460) and mercury (II) concentration was constructed with a linearity of 0-1000 µg L-1. The limit of detection (LOD) and limit of quantification (LOQ) were found at 18.0 µg L-1 and 62.0 µg L-1, respectively. The recovery percentage was in the range of 96.8-106.4%. The developed method was also compared with the standard ICP-OES method. The results were found to be not significantly different at a 95% confidence level (tstat = 0.365 < tcrit = 2.262). This demonstrated that the developed method could be applied for detecting mercury (II) in natural water samples.


Assuntos
Mercúrio , Nanopartículas Metálicas , Água , Espectrometria de Fluorescência/métodos , Cobre , Limite de Detecção , Corantes Fluorescentes
3.
ACS Omega ; 7(30): 26582-26590, 2022 Aug 02.
Artigo em Inglês | MEDLINE | ID: mdl-35936441

RESUMO

Chitosan-grafted thymol (CST) coated on gold nanoparticles has been synthesized and characterized for the design of antimicrobial materials. CST was synthesized via adapting the Mannich reaction, and it acted as the capping agent for the synthesis of gold nanoparticles (AuNPs). The grafting of thymol onto the side chain of chitosan has provided a degree of substitution value (%DSNMR) of 10.0%, calculated by nuclear magnetic resonance spectroscopy. UV-visible spectrometry and elemental analysis were used to confirm the successful synthesis of CST through adapting the Mannich reaction. The appropriate concentration of CST for AuNP synthesis was found to be 0.020%w/v. A red-wine colloidal AuNP solution of 2.41-3.30 nM particle size exhibits a strong surface plasmon resonance at 502 nm, which shows negative charges at pH = 9 of -36.37 mV. This result evidenced that the AuNPs showed electrostatic repulsion and CST played a role as a capping agent to provide a good dispersion and stability state. CST coated on the AuNP surface was successfully utilized for the control of cariogenic bacteria in the oral cavity. The results obtained from this study show that the tuning of the capping agent used in the synthesis step strongly influences the latter antimicrobial activity of the nanoparticles against Streptococcus mutans ATCC 25175 and Streptococcus sobrinus ATCC 33402 activity, with an inhibition zone of 15.90 and 14.25 mm, respectively. The average minimum inhibitory concentration values against S. mutans ATCC 25175 and S. sobrinus ATCC 33402 were found to be 25 and 100 mg/L, respectively, whereas the minimum bactericidal concentration values were 100 and 200 mg/L, respectively.

4.
Molecules ; 25(19)2020 Sep 27.
Artigo em Inglês | MEDLINE | ID: mdl-32992632

RESUMO

A new colorimetric sensor based on gold/silver bimetallic nanoparticles (Au-Ag BNPs) for the sensitive and selective detection of mercury (II) was developed. Gold nanoparticles (AuNPs) were synthesized by Turkevich method. The surface modification of AuNPs was modified by the layer-by-layer technique using poly(diallyl dimethylammonium chloride) which provided positively charged of AuNPs. Negatively charged silver nanoparticles (AgNPs) were synthesized by chemical reduction using poly(4-styrenesulfonic acid-co-maleic acid) as the stabilizing agent. The layer-by-layer assembly deposition technique was used to prepare Au-Ag BNPs of positively and negatively charged of AuNPs and AgNPs, respectively. The synthesized Au-Ag BNPs were characterized by a UV-visible spectrophotometer, zeta potential analyzer, FT-IR, TEM, XRD, and EDX. The Au-Ag BNPs sensor was able to detect mercury (II) in aqueous solution, visibly changing from brownish-orange to purple. The linear relationships of the UV-visible spectrometry demonstrate that the Au-Ag BNPs-based colorimetric sensor can be used for the quantitative analysis of mercury (II) in the range of 0.5-80 mg L-1, with the correlation coefficient, r2 = 0.9818. The limit of detection (LOD) of mercury (II) was found to be 0.526 + 0.001 mg L-1. The BNPs is also verified to have a good practical applicability for mercury (II) detection in the real samples.


Assuntos
Ouro/química , Mercúrio/análise , Nanopartículas Metálicas/química , Prata/química , Colorimetria
5.
Talanta ; 210: 120675, 2020 Apr 01.
Artigo em Inglês | MEDLINE | ID: mdl-31987195

RESUMO

In this work, a microfluidic paper-based analytical device (µPAD) for simultaneous multiple-point standard addition assay was fabricated by rubber stamping the hydrophobic barrier pattern onto a laboratory filter paper. The µPAD has a central zone from which an applied sample flows into eight surrounding narrow channels to which had been added the standard solutions. Each channel is connected to a circular area loaded with the reagent. The opposite end of this reagent zone is connected by second narrow channel to the final circular detection zone. The µPAD was applied to the measurement of creatinine in human urine. After addition of a urine sample, the orange-colored product arising from the Jaffé reaction is formed at the eight detection zones. A digital image of the µPAD is then recorded and the ratio of the red/green (R/G) intensity obtained using the ImageJ™ program is used in the quantitation of creatinine. The normal standard addition calibration line is constructed using the intensity ratio against the added creatinine concentrations (50-1000 mg L-1). Good linearity was achieved (r2 ˃ 0.99). There were no significant differences between the creatinine content using an HPLC method (paired t-test at 95% confidence, tstat = 1.78, tcritical = 2.26, n = 10). The use of simultaneous multiple-point standard addition calibration allows rapid determination of creatinine in urine with elimination of matrix interference.


Assuntos
Creatinina/urina , Técnicas Analíticas Microfluídicas , Papel , Humanos
6.
Anal Sci ; 34(2): 169-175, 2018.
Artigo em Inglês | MEDLINE | ID: mdl-29434102

RESUMO

A new design of membraneless gas-diffusion unit with dual acceptor channels for separation, collection and simultaneous determination of two volatile analytes in liquid sample is presented. The unit is comprised of three parallel channels in a closed module. A sample is aspirated into the central channel and two kinds of reagents are introduced into the other two channels. Two analytes are isolated from the sample matrix by diffusion into head-space and absorbed into the specific reagents. Non-absorbed vapor is released by opening the programmable controlled lid. The unit was applied to liquors for measurement of ethanol and acetaldehyde using reverse flow injection. Dichromate and nitroprusside were exploited as reagents for colorimetric detection of ethanol and acetaldehyde, respectively. Good linearity ranges (r2 >0.99) with high precision (RSD <2%) and high accuracy (recovery: 90 - 105%) were achieved. The results were compared to the results by GC-FID and no significant difference was observed by paired t-test (95% confidence).

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