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1.
Mikrochim Acta ; 190(4): 112, 2023 03 04.
Artículo en Inglés | MEDLINE | ID: mdl-36869922

RESUMEN

For sensitive detection of the L-fuculokinase genome related to the Haemophilus influenzae (H. influenzae), this research work demonstrates the label-free electrochemical-based oligonucleotide genosensing assay relying on the performing hybridization process. To enhance the electrochemical responses, multiple electrochemical modifier-tagged agents were effectively utilized. For attaining this goal, NiCr-layered double hydroxide (NiCr LDH) has been synthesized and combined with biochar (BC) to create an efficient electrochemical signal amplifier that has been immobilized on the surface of the bare Au electrode. Low detection and quantification limits (LOD and LOQ) associated with the designed genosensing bio-platform to detect L-fuculokinase have been achieved to 6.14 fM and 11 fM, respectively. Moreover, the wide linear range of 0.1 to 1000 pM demonstrates the capability of the designed platform. Investigated were the 1-, 2-, and 3-base mismatched sequences, and the negative control samples clarified the high selectivity and better performance of the engineered assay. The values of 96.6-104% and 2.3-3.4% have been obtained for the recoveries and RSDs, respectively. Furthermore, the repeatability and reproducibility of the associated bio-assay have been studied. Consequently, the novel method is appropriate for rapidly and quantitatively detecting H. influenzae, and is considered a better candidate for advanced tests on biological samples such as urine samples.


Asunto(s)
Haemophilus influenzae , Sistemas de Atención de Punto , Reproducibilidad de los Resultados , Amplificadores Electrónicos , Bioensayo
2.
Mikrochim Acta ; 188(3): 100, 2021 02 24.
Artículo en Inglés | MEDLINE | ID: mdl-33629168

RESUMEN

An innovative label-free DNA genosensing assay based on a direct hybridization followed by DPASV in the presence of [Fe(CN)6]4-/3- was developed for recognizing the H. influenza genome in human plasma samples. To attain this objective, Zn-based MOF was synthesized and combined with carboxymethyl cellulose (CMC), which were immobilized on the surface of Au electrode and AuNPs were immobilized on the Zn-based MOF/CMC/Au-modified electrode surface. The genosensing bio-assay provides high specificity, sensitivity, and good performance for the determination of L-fuculokinase gene from the Haemophilus influenza genome. Various characterization techniques were applied including Fe-SEM, EDS, FT-IR, and XRD for investigation of morphological features and particle size. Under optimal conditions LOD and LOQ were 1.48 fM and 3.23 fM, respectively. Moreover, a wide linear range was obtained ranging from 0.1 pM-10 nM for t-DNA. The recoveries and RSDs were 98.4-103% and 2.2-3.2, respectively. The fabricated biosensing assay presented high selective ability of one, two, and three-base mismatched sequences. In addition, negative control of the genosensing assay for investigation of the selectivity was performed by the t-DNAs of Salmonella typhimurium and Shigella flexneri bacteria. Likewise, reproducibility and repeatability of the related bio-assay were investigated. It is to be noted that the organized genosensing bio-assay can be straightforwardly reused and regenerated to assess the hybridization process.


Asunto(s)
Técnicas Biosensibles/métodos , ADN Bacteriano/sangre , Técnicas Electroquímicas/métodos , Haemophilus influenzae/química , Estructuras Metalorgánicas/química , ADN Bacteriano/genética , ADN de Cadena Simple/química , ADN de Cadena Simple/genética , Oro/química , Haemophilus influenzae/enzimología , Humanos , Límite de Detección , Nanopartículas del Metal/química , Hibridación de Ácido Nucleico , Fosfotransferasas (Aceptor de Grupo Alcohol)/genética , Reproducibilidad de los Resultados , Zinc/química
3.
Anal Bioanal Chem ; 412(21): 5053-5065, 2020 Aug.
Artículo en Inglés | MEDLINE | ID: mdl-31897559

RESUMEN

In this work, a novel strategy was introduced to develop a non-enzymatic hydrogen peroxide (H2O2) sensor based on rifampicin (RIF) electrodeposited on a polyvinylpyrrolidone (PVP)-capped CdSe quantum dot (CdSeQD), CoFe2O4 magnetic nanoparticle-modified glassy carbon electrode (CoFe2O4@CdSeQDs/RIF/GCE). CoFe2O4@CdSeQD magnetic nanocomposite (CoFe2O4@CdSeQD MNCs) was synthesized by a chemical co-precipitation method and characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), Fourier-transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). To prepare the non-enzymatic H2O2 sensor, firstly, the glassy carbon electrode surface was modified by dropping 10 µL of 5 mg mL-1 CoFe2O4@CdSeQD MNCs. Then, rifampicin was electrodeposited on the activated CoFe2O4@CdSeQDs/GCE by applying a potential of - 0.7 V for 400 s in pH 2.0 phosphate buffer containing 190 µM of rifampicin. Cyclic voltammetry and electrochemical impedance spectroscopy was used to investigate the electrochemical behavior of this sensor and was used for the reduction of H2O2. Construction of the calibration plot for H2O2 was performed using an amperometric method (- 0.2 V vs. Ag/AgCl) at the modified electrode. Two linearity ranges were obtained from 7 to 145 µM and 145 µM to 1.43 mM with sensitivities of 143.01 µA mM-1 and 28.67 µA mM-1 for the first and second linearity ranges, respectively. The detection limit was obtained as 0.38 µM (S/N = 3). Finally, the reliability of the nanosensor was confirmed with real sample analysis in different beverages such as juice and milk with satisfactory recovery results.


Asunto(s)
Compuestos de Cadmio/química , Cobalto/química , Compuestos Férricos/química , Peróxido de Hidrógeno/análisis , Nanocompuestos/química , Puntos Cuánticos/química , Rifampin/química , Compuestos de Selenio/química , Electrodos , Límite de Detección , Magnetismo , Microscopía Electrónica de Rastreo , Análisis Espectral/métodos , Difracción de Rayos X
4.
J AOAC Int ; 97(1): 252-8, 2014.
Artículo en Inglés | MEDLINE | ID: mdl-24672886

RESUMEN

Simultaneous spectrophotometric determination of three neonicotinoid insecticides (acetamiprid, imidacloprid, and thiamethoxam) by a novel method named generalized net analyte signal standard addition method (GNASSAM) in some binary and ternary synthetic mixtures was investigated. For this purpose, standard addition was performed using a single standard solution consisting of a mixture of standards of all analytes. Savings in time and amount of used materials are some of the advantages of this method. All determinations showed appropriate applicability of this method with less than 5% error. This method may be applied for linearly dependent data in the presence of known interferents. The GNASSAM combines the advantages of both the generalized standard addition method and net analyte signal; therefore, it may be a proper alternative for some other multivariate methods.


Asunto(s)
Imidazoles/química , Insecticidas/química , Nitrocompuestos/química , Oxazinas/química , Piridinas/química , Espectrofotometría/métodos , Tiazoles/química , Contaminantes Ambientales/química , Análisis Factorial , Neonicotinoides , Tiametoxam
5.
Bioimpacts ; 14(3): 28854, 2024.
Artículo en Inglés | MEDLINE | ID: mdl-38938755

RESUMEN

Introduction: The endothelial cells derived from the human vein cord (HUVECs) are used as in-vitro models for studying cellular and molecular pathophysiology, drug and hormones transport mechanisms, or pathways. In these studies, the proliferation and quantity of cells are important features that should be monitored and assessed regularly. So rapid, easy, noninvasive, and inexpensive methods are favorable for this purpose. Methods: In this work, a novel method based on fast Fourier transform square-wave voltammetry (FFTSWV) combined with a 3D printed electrochemical cell including two inserted platinum electrodes was developed for non-invasive and probeless rapid in-vitro monitoring and quantification of human umbilical vein endothelial cells (HUVECs). The electrochemical cell configuration, along with inverted microscope images, provided the capability of easy use, online in-vitro monitoring, and quantification of the cells during proliferation. Results: HUVECs were cultured and proliferated at defined experimental conditions, and standard cell counts in the initial range of 12 500 to 175 000 were prepared and calibrated by using a hemocytometer (Neubauer chamber) counting for electrochemical measurements. The optimum condition, for FFTSWV at a frequency of 100 Hz and 5 mV amplitude, were found to be a safe electrochemical measurement in the cell culture medium. In each run, the impedance or admittance measurement was measured in a 5 seconds time window. The total measurements were fulfilled at 5, 24, and 48 hours after the seeding of the cells, respectively. The recorded microscopic images before every electrochemical assay showed the conformity of morphology and objective counts of cells in every plate well. The proposed electrochemical method showed dynamic linearity in the range of 12 500-265 000 HUVECs 48 hours after the seeding of cells. Conclusion: The proposed electrochemical method can be used as a simple, fast, and noninvasive technique for tracing and monitoring of HUVECs population in in-vitro studies. This method is highly cheap in comparison with other traditional tools. The introduced configuration has the versatility to develop electrodes for the study of various cells and the application of other electrochemical designations.

6.
Sci Rep ; 13(1): 12188, 2023 Jul 27.
Artículo en Inglés | MEDLINE | ID: mdl-37500942

RESUMEN

In the present study, ZnMnFeO4 and CoMnFeO4 tri-metallic spinel oxide nanoparticles (NPs) were provided using hydrothermal methods. The nanoparticles have been characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), Fourier transform infrared spectroscopy (FTIR), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), and electrochemical techniques. A reliable and reproducible electrochemical sensor based on ZnMnFeO4/CoMnFeO4/FTO was fabricated for rapid detection and highly sensitive determination of hydrazine by the DPV technique. It is observed that the modified electrode causes a sharp growth in the oxidation peak current and a decrease in the potential for oxidation, contrary to the bare electrode. The cyclic voltammetry technique showed that there is high electrocatalytic activity and excellent sensitivity in the suggested sensor for hydrazine oxidation. Under optimal experimental conditions, the DPV method was used for constructing the calibration curve, and a linear range of 1.23 × 10-6 M to 1.8 × 10-4 M with a limit of detection of 0.82 ± 0.09 µM was obtained. The obtained results indicate that ZnMnFeO4/CoMnFeO4/FTO nano sensors exhibit pleasant stability, reproducibility, and repeatability in hydrazine measurements. In addition, the suggested sensor was efficiently employed to ascertain the hydrazine in diverse samples of cigarette tobacco.

7.
ACS Omega ; 8(1): 1702-1709, 2023 Jan 10.
Artículo en Inglés | MEDLINE | ID: mdl-36643503

RESUMEN

The ever-expanding human societies on the one hand and the diminishing fossil fuel resources on the other have driven man to find a suitable, cheap, clean, and accessible source of energy. Water splitting is a good solution to this crisis. Because of the slow kinetics of water oxidation reaction, it is important to select efficient and durable electrocatalysts to improve the reaction kinetics. In this research, α-MnO2/FeCo-LDH catalysts on nickel foam were developed for water oxidation, which exhibited good catalytic performance and stability in a 0.1 M KOH solution. The electrocatalysts were synthesized by hydrothermal methods and characterized by XRD, FTIR, Raman, SEM, TEM, EDS, and MAP techniques. The proposed modified electrode has large exchange current, low overpotential, and small Tafel slope. Here, only an overpotential of 210 mV is required to achieve a current density of 5 mA cm2 with a Tafel slope of 70.4 mV dec-1 in an alkaline solution.

8.
Talanta ; 253: 123928, 2023 Feb 01.
Artículo en Inglés | MEDLINE | ID: mdl-36126525

RESUMEN

A two-step and fast electrochemical approach for the synthesis of CdSe@ Cu2Se core-shell quantum dots is applied in the mixture of ethylene glycol-based deep eutectic solvent and 5% water as a green media to modify the graphene film-coated glassy carbon electrode for fabricating a sensitive surface. The quantum dots particles were systematically characterized by Energy-dispersive X-ray spectroscopy (EDS), scanning electron microscopy (SEM), X-ray diffraction (XRD), FT-IR spectroscopy, UV-visible and Fluorescence emission spectroscopy, transmission electron microscopy (TEM) and cyclic voltammetry (CV) techniques. The results show the existence of a second-order chemical reaction after occurring the electron transfer reaction for pyrazinamide. The CdSe@Cu2Se modified graphene-coated glassy carbon electrode was successfully used for the determination of pyrazinamide by differential pulse voltammetry method under the optimized conditions (pH = 2) in the range of 0.4-10 µM with a corresponding detection limit of 0.37 µM. The proposed modified sensor demonstrated high selectivity, reproducibility, stability in the pharmaceutical tablets, urine, and human blood serum and high recoveries in the range of 97.9-101.9% were obtained.


Asunto(s)
Compuestos de Cadmio , Grafito , Compuestos de Selenio , Humanos , Disolventes Eutécticos Profundos , Solventes , Pirazinamida , Reproducibilidad de los Resultados , Espectroscopía Infrarroja por Transformada de Fourier
9.
Heliyon ; 9(6): e16888, 2023 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-37332932

RESUMEN

Bimetallic Ru-Ni nanoparticles was synthesized on the reduced graphene oxide decorated Ni foam (Ru-Ni/rGO/NF) by electroplating method to be utilized as the anode electrocatalyst for direct hydrazine-hydrogen peroxide fuel cells (DHzHPFCs). The synthesized electrocatalysts were characterized by X-ray diffraction, Field emission scanning electron microscopy, Fourier transform infrared spectroscopy, and Raman spectroscopy. The electrochemical properties of catalysts towards hydrazine oxidation reaction in an alkaline medium were evaluated by cyclic voltammetry, chronoamperometry, and electrochemical impedance spectroscopy. In the case of Ru1-Ni3/rGO/NF electrocatalyst, Ru1-Ni3 provided active sites due to low activation energy (22.24 kJ mol-1) for hydrazine oxidation reaction and reduced graphene oxide facilitated charge transfer by increasing electroactive surface area (EASA = 677.5 cm2) with the small charge transfer resistance (0.1 Ω cm2). The CV curves showed that hydrazine oxidation on the synthesized electrocatalysts was a first-order reaction in low concentrations of N2H4 and the number of exchanged electrons was 3.0. In the single cell of the of direct hydrazine-hydrogen peroxide fuel cell, the maximum power density value of Ru1-Ni3/rGO/NF electrocatalyst was 206 mW cm-2 and the open circuit voltage was 1.73 V at 55 °C. These results proved that the Ru1-Ni3/rGO/NF is a promising candidate for using as the free-binder anode electrocatalyst in the future application of direct hydrazine-hydrogen peroxide fuel cells due to its excellent structural stability, ease of synthesis, low cost, and high catalytic performance.

10.
Environ Monit Assess ; 184(2): 1089-96, 2012 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-21484298

RESUMEN

A differential pulse polarography (DPP) for the simultaneous determination of 2-nitrophenol and 4-nitrophenol was proposed. It was found that under optimum experimental conditions (pH = 5, scan rate = 5 mV/s, pulse amplitude = -50 mV), 2-nitrophenol and 4-nitrophenol had well-defined polarographic reduction waves with peak potentials at -317 and -406 mV, respectively. In the mixture of two compounds overlapping polarographic peaks were observed. In this study, support vector regression (SVR) was applied to resolve the overlapped polarograms. Furthermore, a comparison was made between the performance of SVR and partial least square (PLS) on data set. The results demonstrated that SVR is a better well-performing alternative for the analysis and modeling of DPP data than the commonly applied PLS technique. The proposed method was used for the determination of 2-nitrophenol and 4-nitrophenol in industrial waste water.


Asunto(s)
Monitoreo del Ambiente/métodos , Nitrofenoles/análisis , Polarografía , Contaminantes Químicos del Agua/análisis , Monitoreo del Ambiente/instrumentación , Residuos Industriales/análisis , Nitrofenoles/química , Contaminantes Químicos del Agua/química
11.
Chemosphere ; 287(Pt 4): 132373, 2022 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-34600005

RESUMEN

Monitoring of pathogenic bacteria plays a vital role in precluding foodborne disease outbreaks. In this research work, a genosensor based on innovative label-free DNA was developed for the detection of Salmonella. typhimurium (S. typhimurium) in the milk samples. To realize this objective, bimetallic Fe/Mn MOF is synthesized and mixed with methyl-ß-cyclodextrin (MßCD) and AuNPs which are then stabilized on multi-walled carbon nanotubes (MWCNTs), and the obtained nanocomposite is immobilized on the Au electrode surface. Different characterization methods such as FE-SEM, TEM, EDS, FTIR, and XRD were used for investigating the particle size and morphological features. Electrochemical and impedimetric techniques were used for exploring the applicability of the fabricated genosensor. Under optimal circumstances, LOD and LOQ have acquired at 0.07 pM and 0.21 pM. Moreover, an extensive linear range of 1 pM-1 µM was resulted for ss-tDNA (single-stranded target DNA), R2 obtained 0.9991. The recoveries were obtained 95.6-104%. Great selectivity against one, two, and three-base mismatched sequences was also shown for fabricated biosensing assay. Furthermore, negative genosensing assay control for investigating selectivity was provided by the ss-tDNAs of Haemophilusinfluenzae and Shigella dysenteriae bacteria. Well-fabricated genosensing bio-assay represents better performance, great specificity, high sensitivity, increased active sites, and finally results in an increase in the electron transfer rate. It is to be noted that the organized genosensing bio-assay is capable of being re-used and re-generated in a straightforward manner to estimate the hybridization process.


Asunto(s)
Técnicas Biosensibles , Nanopartículas del Metal , Nanotubos de Carbono , Animales , ADN , Técnicas Electroquímicas , Oro , Límite de Detección , Leche , Salmonella typhimurium/genética , beta-Ciclodextrinas
12.
Chemosphere ; 288(Pt 2): 132531, 2022 Feb.
Artículo en Inglés | MEDLINE | ID: mdl-34653485

RESUMEN

Shigella dysenteriae, a gram-negative bacterium, which results in the most infectious of bacterial shigellosis and dysenteries. In this study, an innovative gene detection platform based on label-free DNA sequences was developed to detect Shigella dysenteriae in human plasma samples. The porous and honeycomb-like structure of biochar (BC) was first synthesized through a pyrolysis process. Then, the produced biochar was effectively decorated with flower-like MoS2 nanosheets (MoS2/BC). The resulting nanocomposite was incorporated with Au nanoparticles (AuNPs) by applying chronoamperometry technique, and then the subsequent product including MoS2 nanosheets, biochar and AuNPs were immobilized on the Au electrode surface and used for modifier agent in electrochemical bio-assays. Structural and morphological study of the synthesized compounds were investigated using various characterization methods such as FE-SEM, TEM, EDS, FTIR, and XRD. Various electrochemical techniques including cyclic voltammetry (CV) and Differential pulse anodic stripping voltammetry (DPASV) have been used to investigate the applicability of the fabricated genosensing bio-assay. Under optimal conditions, LOD and LOQ were calculated 9.14 fM and 0.018 pM respectively. In addition, a linear range from 0.01 to 100 pM was obtained for single stranded-target DNA (ss-tDNA), with R2 of 0.9992. The recoveries ranged from 98.0 to 101.3%. The fabricated bio-detection assay demonstrated high selectivity for 1, 2, and 3 base mismatch sequences. In addition, a negative control of the gene detection platform which was performed to study selectivity was provided by ss-tDNA from Haemophilusinfluenzae, and Salmonella typhimurium. Moreover, it is important to mention that the organized bioassay is simply reusable and reproducible with the RSD% (relative standard deviation) ˂ 5 to next detection assays.


Asunto(s)
Oro , Nanopartículas del Metal , Carbón Orgánico , Humanos , Molibdeno , Porosidad , Shigella dysenteriae
13.
J AOAC Int ; 93(6): 1995-2001, 2010.
Artículo en Inglés | MEDLINE | ID: mdl-21313830

RESUMEN

A novel net analyte signal standard addition method (NASSAM) was used for simultaneous determination of the drugs anthazoline and naphazoline. The NASSAM can be applied for determination of analytes in the presence of known interferents. The proposed method is used to eliminate the calibration and prediction steps of multivariate calibration methods; the determination is carried out in a single step for each analyte. The accuracy of the predictions against the H-point standard addition method is independent of the shape of the analyte and interferent spectra. The net analyte signal concept was also used to calculate multivariate analytical figures of merit, such as LOD, selectivity, and sensitivity. The method was successfully applied to the simultaneous determination of anthazoline and naphazoline in a commercial eye drop sample.


Asunto(s)
Agonistas alfa-Adrenérgicos/análisis , Antazolina/análisis , Antialérgicos/análisis , Nafazolina/análisis , Algoritmos , Calibración , Combinación de Medicamentos , Concentración de Iones de Hidrógeno , Indicadores y Reactivos , Soluciones Oftálmicas/análisis , Soluciones , Espectrofotometría Ultravioleta
14.
Comb Chem High Throughput Screen ; 23(10): 1023-1031, 2020.
Artículo en Inglés | MEDLINE | ID: mdl-32436826

RESUMEN

AIM AND OBJECTIVE: Methyldopa is one of the medications that is used for the treatment of hypertension. Therefore, the determination of methyldopa in the presence of other biological components is essential. In this work, a promising electrochemical sensor based on CoFe2O4 magnetic nanoparticles modified glassy carbon electrode (CoFe2O4/GCE) was developed for electrochemical determination of methyldopa in the presence of uric acid. Cobalt ferrite nanoparticles were synthesized via chemical method. MATERIALS AND METHODS: Characterizing the CoFe2O4 was investigated by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), energy dispersive X-ray spectroscopy (EDX), transmission electron microscope (TEM), and cyclic voltammetry techniques. RESULTS: Under the optimal experimental conditions, the current response of the electrochemical sensor obtained with differential pulse voltammetry was increased linearly in the concentration range from 1.45 to 15.1 µmol L-1 with the detection limit of 1.07 µmol L-1 for methyldopa. Also, by using the proposed method, methyldopa and uric acid could be analyzed in a mixture independently. The difference in peak potential for analytes is about 150 mV. CONCLUSION: The present sensor was successfully applied for the determination of methyldopa in the presence of uric acid in biological samples and the pharmaceutical samples with satisfactory results.


Asunto(s)
Técnicas Biosensibles , Cobalto/química , Técnicas Electroquímicas , Compuestos Férricos/química , Metildopa/análisis , Nanopartículas/química , Ácido Úrico/química , Electrodos , Compuestos Férricos/síntesis química , Humanos , Fenómenos Magnéticos , Tamaño de la Partícula , Propiedades de Superficie , Comprimidos
15.
J AOAC Int ; 92(2): 548-54, 2009.
Artículo en Inglés | MEDLINE | ID: mdl-19485215

RESUMEN

A sol-gel carbon ceramic electrode (CCE) without any assigned electron transfer mediator or specific reagents was used for the determination of fenitrothion by square-wave adsorptive stripping voltammetry. Fenitrothion strongly adsorbs on a CCE surface, which enables the development of facile electrochemical quantitative methods. Operational parameters such as pH value, initial potential value, and pulse frequency were optimized, and the stripping voltammetric performance was studied by using square-wave voltammetry. Square-wave adsorptive stripping voltammetry was used to obtain calibration curves with 2 linear ranges, 0.005-0.1 and 0.1-50 microM; the lower linear range was used to calculate the detection limit, 0.0016 microM (5 min adsorption). The effect of interference species on the determination of fenitrothion was also studied. The inherent stability, high sensitivity, low detection limit, and low cost of analysis are the advantages of this sensor. The present method was successfully applied to the determination of fenitrothion in a commercial formulation and river water samples. Analysis of real water samples by using the sensor demonstrated the feasibility of applying the sensor to the on-site monitoring of organophosphate compounds.


Asunto(s)
Técnicas Electroquímicas/métodos , Fenitrotión/análisis , Plaguicidas/análisis , Contaminantes Químicos del Agua/análisis , Carbono , Cerámica , Técnicas Electroquímicas/estadística & datos numéricos , Electrodos , Ríos/química , Sensibilidad y Especificidad
16.
J AOAC Int ; 92(6): 1807-14, 2009.
Artículo en Inglés | MEDLINE | ID: mdl-20166599

RESUMEN

The net analyte preprocessing/classical least-squares (NAP/CLS) method is a simple chemometric method that has been used for the simultaneous spectrophotometric determination of benzoic acid, sorbic acid, and ascorbic acid. The obtained results indicated that the performances of the NAP/CLS and partial least-squares methods were almost identical. The net analyte signal (NAS) concept was also used to calculate multivariate analytical figures of merit, such as LOD, selectivity, and sensitivity. Wavelength selection was applied based on the concept of NAS regression, and improved the method performance in samples containing nonmodeled interferences. The method afforded recoveries in the range of 98-105%. The proposed method was successfully applied to determination of the analytes in an Iranian soft drink.


Asunto(s)
Ácido Ascórbico/análisis , Ácido Benzoico/análisis , Conservantes de Alimentos/análisis , Ácido Sórbico/análisis , Algoritmos , Bebidas/análisis , Calibración , Indicadores y Reactivos , Análisis de los Mínimos Cuadrados , Análisis Multivariante , Reproducibilidad de los Resultados , Programas Informáticos , Soluciones , Espectrofotometría Ultravioleta
17.
J Sep Sci ; 31(21): 3788-95, 2008 Dec.
Artículo en Inglés | MEDLINE | ID: mdl-18956382

RESUMEN

The depicted retention times (RTs) of an electron capture detection (ECD) system is predicted for a set of 37 pentafluorobenzyl (PFB) derivatives of phenol in a semi-polar column, DB-1701 (14% cyanopropylphenyl and 86% dimethyl-polysiloxane). Among a large number of descriptors, four parameters categorized as electronic, topological, geometric, and hybrid (geometric and topological) descriptors are chosen using stepwise multiple regression technique. Each molecular descriptor in this model was disputed to unfold the relationship between molecular structures and their RTs. The descriptors occurring in the multiple linear regression (MLR) model were considered as inputs for developing the back propagation artificial neural networks (BPANN). The artificial neural network (ANN) model shows superiority over the MLR by decerning 91.9% for different classes of molecules in confusion matrix. This refers to the fact that the retention behaviors of molecules display nonlinear characteristics. The accuracy of 4-4-1 BPANN model was illustrated using leave-one-out (LOO), leave-multiple-out (LMO) cross-validations, and Y-randomization. Moreover, the mean effect of descriptors betrays that descriptor Ss is the most indispensable factor affecting the retention behavior of molecules.

18.
Anal Chim Acta ; 1011: 28-34, 2018 Jun 29.
Artículo en Inglés | MEDLINE | ID: mdl-29475482

RESUMEN

A new label-free electrochemical immunosensor is constructed for the selective and sensitive determination of the clinically relevant biomarker receptor tyrosine kinase (AXL) in human serum. The disposable immunosensing platform is prepared by immobilization of the specific anti-AXL antibody onto amine functionalized graphene quantum dots (fGQDs)-modified screen-printed carbon electrodes (SPCEs). The affinity reactions were monitored by measuring the decrease in the differential pulse voltammetric (DPV) response of the redox probe Fe(CN)63-/4-. All the experimental variables involved in the preparation of the modified electrodes and in the immunosensor performance were optimized. The as prepared immunosensor exhibits an improved analytical performance with respect to other electrochemical immunosensors reported so far, with a wider range of linearity and a lower detection limit, 0.5 pg mL-1, which is more than one hundred thousand times lower than the established cut-off value for heart failure (HF) diagnosis in serum (71 ng mL-1). The developed immunosensor was successfully applied to the determination of the endogenous content of AXL in serum of HF patients without any matrix effect observed after just a sample dilution.


Asunto(s)
Grafito/química , Impresión , Proteínas Proto-Oncogénicas/sangre , Puntos Cuánticos/química , Proteínas Tirosina Quinasas Receptoras/sangre , Biomarcadores/sangre , Técnicas Electroquímicas , Electrodos , Humanos , Inmunoensayo , Tamaño de la Partícula , Propiedades de Superficie , Tirosina Quinasa del Receptor Axl
19.
Biosens Bioelectron ; 92: 509-516, 2017 Jun 15.
Artículo en Inglés | MEDLINE | ID: mdl-27840036

RESUMEN

This work introduces a new electrochemical sensor based on polyvinyl pyrrolidone capped CoFe2O4@CdSe core-shell modified electrode for a rapid detection and highly sensitive determination of rifampicin (RIF) by square wave adsorptive stripping voltammetry. The new PVP capped CoFe2O4@CdSe with core-shell nanostructure was synthesized by a facile synthesis method for the first time. PVP can act as a capping and etching agent for protection of the outer surface nanoparticles and formation of a mesoporous shell, respectively. Another important feature of this work is the choice of the ligand (1,10-phenanthroline) for precursor cadmium complex that works as a chelating agent in order to increase optical and electrical properties and stability of prepared nanomaterial. The nanoparticles have been characterized by field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), energy dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), UV-vis, photoluminescence (PL) spectroscopy, FT-IR, and cyclic voltammetry techniques. The PL spectroscopy study of CoFe2O4@CdSe has shown significant PL quenching by the formation of CoFe2O4 core inside CdSe, this shows that CoFe2O4 NPs are efficient electron acceptors with the CdSe. It is clearly observed that the biosensor can significantly enhance electrocatalytic activity towards the oxidation of RIF, under the optimal conditions. The novelty of this work arises from the new synthesis method for the core-shell of CoFe2O4@CdSe. Then, the novel electrochemical biosensor was fabricated for ultra-trace level determination of rifampicin with very low detection limit (4.55×10-17M) and a wide linear range from 1.0×10-16 to 1.0×10-7M. The fabricated biosensor showed high sensitivity and selectivity, good reproducibility and stability. Therefore, it was successfully applied for the determination of ultra-trace RIF amounts in biological and pharmaceutical samples with satisfactory recovery data.


Asunto(s)
Antibióticos Antituberculosos/sangre , Compuestos de Cadmio/química , Cobalto/química , Técnicas Electroquímicas/instrumentación , Compuestos Férricos/química , Nanopartículas/química , Povidona/química , Rifampin/sangre , Compuestos de Selenio/química , Antibióticos Antituberculosos/análisis , Técnicas Biosensibles/instrumentación , Humanos , Leprostáticos/análisis , Leprostáticos/sangre , Límite de Detección , Nanopartículas/ultraestructura , Reproducibilidad de los Resultados , Rifampin/análisis , Comprimidos
20.
Iran J Pharm Res ; 15(4): 713-723, 2016.
Artículo en Inglés | MEDLINE | ID: mdl-28243267

RESUMEN

Three antituberculosis medications are investigated in this work consist of rifampicin, isoniazid and pyrazinamide. The ultra violet (UV) spectra of these compounds are overlapped, thus use of suitable chemometric methods are helpful for simultaneous spectrophotometric determination of them. A generalized version of net analyte signal standard addition method (GNASSAM) was used for determination of three antituberculosis medications as a model system. In generalized net analyte signal standard addition method only one standard solution was prepared for all analytes. This standard solution contains a mixture of all analytes of interest, and the addition of such solution to sample, causes increases in net analyte signal of each analyte which are proportional to the concentrations of analytes in added standards solution. For determination of concentration of each analyte in some synthetic mixtures, the UV spectra of pure analytes and each sample were recorded in the range of 210 nm-550 nm. The standard addition procedure was performed for each sample and the UV spectrum was recorded after each addition and finally the results were analyzed by net analyte signal method. Obtained concentrations show acceptable performance of GNASSAM in these cases.

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