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1.
Talanta ; 238(Pt 1): 123031, 2022 Feb 01.
Artículo en Inglés | MEDLINE | ID: mdl-34857349

RESUMEN

In this work, gel electro-membrane extraction (G-EME) combined with flame atomic absorption spectrometry (FAAS) was used for the determination of zinc ions (Zn2+) in water samples. For the first time, the effect of the presence of three types of complexing agents such as phenanthroline (Phen), crown ethers (12C4, 15C5, 18C6), and ethylene-diamine-tetra-acetic acid (EDTA) on the extraction efficiency of zinc ions was studied. In addition, the electroendosmosis (EEO) flow as an unwanted actuator was monitored in the presence and absence of complexing agents. By applying 50 V electrical potential across the membrane, the positive charged Zn2+ ions were migrated from a donor phase (pH 5.0) through the agarose gel membrane (pH 5.0, containing a complexing agent) into the acceptor phase (pH 3.0). The obtained results showed that the highest extraction recoveries were obtained when crown ethers, especially 1% (w/v) 18C6 was added to the gel membrane. In addition, EEO flow was decreased in the presence of all complexing agents (except EDTA), probably due to the increase in electrical resistance. Using the optimum conditions, the limit of detection (LOD), the limit of quantification (LOQ), and extraction recovery% (ER%) were 5.0 µg L-1, 15.0 µg L-1, and 92.5%, respectively. In the end, the applicability of the developed approach was successfully evaluated to determine Zn2+ in tap, mineral, and river water samples.


Asunto(s)
Agua Dulce , Zinc , Concentración de Iones de Hidrógeno , Iones , Espectrofotometría Atómica , Agua
2.
Mol Divers ; 25(1): 509-516, 2021 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-31919737

RESUMEN

Electro-synthesis through a one-pot three-component condensation of corresponding aldehydes, Meldrum's acid, and 2-(nitromethylene)imidazolidine resulted in a series of novel tetrahydroimidazo[1,2-a]pyridine-5(1H)-one derivatives containing an electronegative pharmacophore (=CNO2). The process was carried out in propanol medium with sodium bromide presented as electrolyte, inside an undivided cell with good to excellent yields. As a powerful entry into fused polycyclic structures related to bioactive heterocycles, this green protocol shows great potential.


Asunto(s)
Técnicas de Química Sintética , Electroquímica/métodos , Piridinas/síntesis química , Dioxanos/química , Piridinas/química
3.
Mol Divers ; 24(3): 763-770, 2020 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-31414305

RESUMEN

Due to the diverse applications of cyclopropane analogs in bioorganic, medicinal, and pharmaceutical chemistry, a clean and efficient procedure was established to synthesize spirocyclopropane via an electrochemical reaction which involves a sequence of Michael addition, halogenation, and intramolecular ring-closing reaction. In this study, an environmentally benign synthesis of spirocyclopropane was carried out through the condensation of indan-1,3-dione by aromatic aldehydes or 2-benzylidenemalononitrile derivatives. Constant current electrosynthesis was applied to a mixture of propanol containing sodium bromide as an electrolyte and a brominating agent at room temperature, respectively.


Asunto(s)
Ciclopropanos/química , Ciclopropanos/síntesis química , Compuestos de Espiro/química , Aldehídos/química , Bromuros/química , Catálisis , Técnicas de Química Sintética , Electroquímica , Tecnología Química Verde , Temperatura
4.
J Biomol Struct Dyn ; 35(3): 603-615, 2017 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-27151742

RESUMEN

In this study, a novel method to probe molecular interactions and binding of human hemoglobin (Hb) with nanodiamond (ND) was introduced based on the surface tension measurement. This method complements conventional techniques, which are basically done by zeta potential and dynamic light scattering (DLS) measurements, near and far circular dichroism (CD) spectroscopy, intrinsic and extrinsic fluorescence spectroscopy. Addition of ND to Hb solution increased the surface tension value of Hb-ND complex relative to those of Hb and ND molecules. The zeta potential values reveled that Hb and ND provide identical charge distribution at pH 7.5. DLS measurements demonstrated that Hb, ND, and ND-Hb complex have hydrodynamic radiuses of 98.37 ± 4.57, 122.07 ± 7.88 nm and 62.27 ± 3.70 at pH of 7.5 respectively. Far and near UV-CD results indicated the loss of α-helix structure and conformational changes of Hb, respectively. Intrinsic fluorescence data demonstrated that the fluorescence quenching of Hb by ND was the result of the static quenching. The hydrophobic interaction plays a pivotal role in the interaction of ND with Hb. Fluorescence intensity changes over time revealed conformational change of Hb continues after the mixing of the components (Hb-ND) till 15 min, which is indicative of the denaturation of the Hb relative to the protein control. Extrinsic fluorescence data showed a considerable enhancement of the ANS fluorescence intensity of Hb-ND system relative to the Hb till 60 nM of ND, likely persuaded by greater exposure of nonpolar residues of Hb hydrophobic pocket. The remarkable decrease in Tm value of Hb in Hb-ND complex exhibits interaction of Hb with ND conducts to conformational changes of Hb. This study offers consequential discrimination into the interaction of ND with proteins, which may be of significance for further appeal of these nanoparticles in biotechnology prosecution.


Asunto(s)
Hemoglobinas/química , Nanodiamantes/química , Análisis Espectral , Tensión Superficial , Dicroismo Circular , Humanos , Concentración de Iones de Hidrógeno , Interacciones Hidrofóbicas e Hidrofílicas , Espectrometría de Fluorescencia , Termodinámica
5.
J Food Drug Anal ; 24(2): 406-416, 2016 04.
Artículo en Inglés | MEDLINE | ID: mdl-28911596

RESUMEN

In the present study, the fabrication of a new modified electrode for electrocatalytic oxidation of noradrenalin, based on the delphinidin immobilized on silver nanoparticles modified glassy carbon electrode. Cyclic voltammetry was used to investigate the redox properties of this modified electrode. The surface charge transfer rate constant (ks) and the charge transfer coefficient (α) for the electron transfer between the glassy carbon electrode and the immobilized delphinidin were calculated. The differential pulse voltammetry exhibited two linear dynamic ranges and a detection limit of 0.40µM for noradrenalin determination. Moreover, the present electrode could separate the oxidation peak potentials of ascorbic acid, noradrenalin, uric acid, and tryptophan in a mixture. The usefulness of this nanosensor was also investigated for the determination of ascorbic acid, noradrenalin, and uric acid in pharmaceutical and biological fluid samples with satisfactory results.


Asunto(s)
Nanopartículas del Metal , Antocianinas , Ácido Ascórbico , Norepinefrina , Oxidación-Reducción , Plata , Triptófano , Ácido Úrico
6.
Mater Sci Eng C Mater Biol Appl ; 33(3): 1491-7, 2013 Apr 01.
Artículo en Inglés | MEDLINE | ID: mdl-23827600

RESUMEN

In the present study, a modified carbon paste electrode (CPE) containing multi-wall carbon nanotubes and an indenedione derivative(IMWCNT-CPE) was constructed and was successfully used for dopamine(DA) electrocatalytic oxidation and simultaneous determination of DA and uric acid (UA). Cyclic voltammograms of the IMWCNT-CPE show a pair of well-defined and reversible redox. The obtained results indicate that the peak potential of DA oxidation at IMWCNT-CPE shifted by about 65 and 185 mV toward the negative values compared with that at a MWCNT and indenedione modified CPE, respectively. The electron transfer coefficient, α, and the heterogeneous electron transfer rate constant, k', for the oxidation of DA at IMWCNT-CPE were calculated 0.4±0.01 and (1.13±0.03)×10(-3) cm s(-1), respectively. Furthermore, differential pulse voltammetry (DPV) exhibits two linear dynamic ranges of 1.9-79.4 µM, and 79.4-714.3 µM and a detection limit of 0.52 µM for DA determination. Then IMWCNT-CPE was applied to the simultaneous determination of DA and UA with DPV. Finally, the activity of the modified electrode was also investigated for determination of DA and UA in real samples, such as injection solution of DA and urine, with satisfactory results.


Asunto(s)
Carbono/química , Dopamina/análisis , Técnicas Electroquímicas/métodos , Indenos/química , Nanotubos de Carbono/química , Ácido Úrico/análisis , Catálisis , Electrodos , Humanos , Concentración de Iones de Hidrógeno , Inyecciones , Oxidación-Reducción , Soluciones , Ácido Úrico/orina
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