Enhanced electrocatalytic activity of fluorine doped tin oxide (FTO) by trimetallic spinel ZnMnFeO4/CoMnFeO4 nanoparticles as a hydrazine electrochemical sensor.

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.

Ru-Ni nanoparticles electrodeposited on rGO/Ni foam as a binder-free, stable and high-performance anode catalyst for direct hydrazine fuel cell.

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.

Self-assembled monolayer-assisted label-free electrochemical genosensor for specific point-of-care determination of Haemophilus influenzae.

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.

α-MnO2/FeCo-LDH on Nickel Foam as an Efficient Electrocatalyst for Water Oxidation.

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.

A deep eutectic solvent-assisted electrochemical synthesis of TGA capped CdSe@Cu2Se core-shell quantum dots on the graphene-modified electrode as a catalytic platform for the determination of pyrazinamide.

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.

Bimetallic Fe/Mn MOFs/MßCD/AuNPs stabilized on MWCNTs for developing a label-free DNA-based genosensing bio-assay applied in the determination of Salmonella typhimurium in milk samples.

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.

A PCR-free genosensing platform for detection of Shigella dysenteriae in human plasma samples by porous and honeycomb-like biochar decorated with ultrathin flower-like MoS2 nanosheets incorporated with Au nanoparticles.

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.

A novel engineered label-free Zn-based MOF/CMC/AuNPs electrochemical genosensor for highly sensitive determination of Haemophilus Influenzae in human plasma samples.

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.

Preparation of A Magnetic Nanosensor Based on Cobalt Ferrite Nanoparticles for The Electrochemical Determination of Methyldopa in The Presence of Uric Acid.

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.

Non-enzymatic monitoring of hydrogen peroxide using novel nanosensor based on CoFe2O4@CdSeQD magnetic nanocomposite and rifampicin mediator.

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.

Ultrasensitive determination of receptor tyrosine kinase with a label-free electrochemical immunosensor using graphene quantum dots-modified screen-printed electrodes.

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.

Novel electrochemical biosensor based on PVP capped CoFe2O4@CdSe core-shell nanoparticles modified electrode for ultra-trace level determination of rifampicin by square wave adsorptive stripping voltammetry.

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.

Evaluation of physicochemical properties and in vivo efficiency of atorvastatin calcium/ezetimibe solid dispersions.

Fixed-dose combination of atorvastatin calcium (ATV) and ezetimibe (EZT) provides a considerable advantage in the management of hyperlipidemia. However, both ATV and EZT suffer from the poor aqueous solubility, which can limit their oral bioavailability. The aim of the present study was to improve the in vitro performance and evaluate the in vivo efficiency of the improved (ATV/EZT) fixed-dose combination. The formulation was prepared through solid dispersion (SD)technique, using Polyvinylpyrrolidone K30 via solvent method. Solid-state analysis and the in vitro drug release of the prepared formulations were also assessed. In order to estimate the therapeutic efficiency of the prepared SDs, in vivo studies including measurement of serum lipid levels, liver index and histological analysis of the liver tissue in hyperlipidemic rats were conducted. Differential scanning calorimetry (DSC) and powder X-ray diffractometry (PXRD) showed that the drugs crystallinity was notably decreased during the preparation process. All SDs showed enhanced release for both drugs compared to their binary mixture, drugs: polymer physical mixtures (PMs) and marketed product. Administration of ATV/EZT SD led to a remarkable decrease (P<0.05) in the serum levels of total cholesterol (TC) and LDL-C in the high fat diet-induced hyperlipidemic rats compared to the PM. Additionally, the histopathological examination of the liver tissue revealed the improved efficiency of the SDs on the liver steatosis. According to the obtained results, ATV/EZT SD with improved physicochemical characteristics, showed favorable effects on the serum lipid levels and liver steatosis.

Simultaneous Spectrophotometric Determination of Rifampicin, Isoniazid and Pyrazinamide in a Single Step.

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.

Second order advantage obtained by spectroelectrochemistry along with novel carbon nanotube modified mesh electrode: Application for determination of acetaminophen in Novafen samples.

A matrix-augmentation multivariate curve resolution-alternating least-squares (MA-MCR-ALS) has been conducted on the spectroelectrochemical data of acetaminophen oxidation in order to quantify acetaminophen in Novafen capsule in the presence of unknown interferences. The experiments were carried out using new cheap mesh electrode, namely carbon nanotube modified mesh electrode (CNMME) as optically transparent thin layer electrode (OTTLE). For each sample, a second order spectroelectrochemical data was obtained and MA-MCR-ALS method was applied to analyze these data. Unlike full trilinear models such as PARAFAC, MCR-ALS is flexible in applying trilinearity constraint for each component, a fact which makes it manage deviations from trilinearity of data effectively. This method was employed in both spectral and kinetic augmentation mode of data under examining different trilinear components. However, spectral augmentation was the only setting which allows MA-MCR-ALS to solve the analytical problem achieving the second order advantage. Therefore, here the results of the augmentation in this mode have been described. In order to obtain the best analytical figures of merit in the analysis, different constraints were investigated. The results indicated the accuracy of the proposed method.

Biodegradation of Para Amino Acetanilide by Halomonas sp. TBZ3.

BACKGROUND: Aromatic compounds are known as a group of highly persistent environmental pollutants. Halomonas sp. TBZ3 was isolated from the highly salty Urmia Lake of Iran. In this study, characterization of a new Halomonas isolate called Halomonas sp. TBZ3 and its employment for biodegradation of para-amino acetanilide (PAA), as an aromatic environmental pollutant, is described. OBJECTIVES: This study aimed to characterize the TBZ3 isolate and to elucidate its ability as a biodegradative agent that decomposes PAA. MATERIALS AND METHODS: Primarily, DNA-DNA hybridization between TBZ3, Halomonas denitrificans DSM18045T and Halomonas saccharevitans LMG 23976T was carried out. Para-amino acetanilide biodegradation was assessed using spectrophotometry and confirmed by gas chromatography-mass spectroscopy (GC-MS). Parameters effective on biodegradation of PAA were optimized by the Response Surface Methodology (RSM). RESULTS: The DNA-DNA hybridization experiments between isolate TBZ3, H. denitrificans and H. saccharevitans revealed relatedness levels of 57% and 65%, respectively. According to GC-MS results, TBZ3 degrades PAA to benzene, hexyl butanoate, 3-methyl-1-heptanol and hexyl hexanoate. Temperature 32.92°C, pH 6.76, and salinity 14% are the optimum conditions for biodegradation with a confidence level of 95% (at level α = 0.05). CONCLUSIONS: According to our results, Halomonas sp. TBZ3 could be considered as a biological agent for bioremediation of PAA and possibly other similar aromatic compounds.

Synthesis of dendritic silver nanostructures supported by graphene nanosheets and its application for highly sensitive detection of diazepam.

In this paper, preparation, characterization and application of a new sensor for fast and simple determination of trace amount of diazepam were described. This sensor is based on Ag nanodendrimers (AgNDs) supported by graphene nanosheets modified glassy carbon electrode (GNs/GCE). The AgNDs were directly electrodeposited on the surface of electrode via potentiostatic method without using any templates, surfactants, or stabilizers. The structure of the synthesized AgNDs/GNs was characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, X-ray diffraction (XRD) and electrochemical impedance spectroscopy (EIS) techniques. The nanodendrimers with tree-like and hierarchical structures have a fascinating structure for fabrication of effective electrocatalysts. The experimental results confirmed that AgNDs/GNs/GC electrode has good electrocatalytic activity toward the reduction of diazepam. A low detection limit of 8.56×10(-8)M and a wide linear detection range of 1.0×10(-7) to 1.0×10(-6)M and 1.0×10(-6) to 20×10(-6)M were achieved via differential pulse voltammetry (DPV). The proposed electrode displayed excellent repeatability and long-term stability and it was satisfactorily used for determination of diazepam in real samples (commercially tablet, injection and human blood plasma) with high recovery.

Generalized net analyte signal standard addition as a novel method for simultaneous determination: application in spectrophotometric determination of some pesticides.

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.

Electrochemical synthesis of nickel-iron layered double hydroxide: application as a novel modified electrode in electrocatalytic reduction of metronidazole.

A new and simple approach based on the electrochemical method was used for preparation of reproducible nanostructure thin film of Ni/Fe-layered double hydroxides (Ni/Fe-LDH) on the glassy carbon electrode (GCE). The electrochemical behavior of the Ni/Fe-LDH deposited on GCE electrode is studied. Study of the scanning electron microscopy shows the formation of a nanostructure thin film on the glassy carbon electrode. Electrochemical experiments show that Ni/Fe-LDH modified glassy carbon electrode exhibits excellent electrocatalytic reduction activity with Metronidazole. The method was successfully applied for the analysis of Metronidazole in tablets. The results were favorably compared to those obtained by the reported BP method.

Analysis of variation matrix array by bilinear least squares-residual bilinearization (BLLS-RBL) for resolving and quantifying of foodstuff dyes in a candy sample.

Bilinear least square (BLLS) method is one of the most suitable algorithms for second-order calibration. Original BLLS method is not applicable to the second order pH-spectral data when an analyte has more than one spectroscopically active species. Bilinear least square-residual bilinearization (BLLS-RBL) was developed to achieve the second order advantage for analysis of complex mixtures. Although the modified method is useful, the pure profiles cannot be obtained and only the linear combination will be obtained. Moreover, for prediction of analyte in an unknown sample, the original algorithm of RBL may diverge; instead of converging to the desired analyte concentrations. Therefore, Gauss Newton-RLB algorithm should be used, which is not as simple as original protocol. Also, the analyte concentration can be predicted on the basis of each of the equilibrating species of the component of interest that are not exactly the same. The aim of the present work is to tackle the non-uniqueness problem in the second order calibration of monoprotic acid mixtures and divergence of RBL. Each pH-absorbance matrix was pretreated by subtraction of the first spectrum from other spectra in the data set to produce full rank array that is called variation matrix. Then variation matrices were analyzed uniquely by original BLLS-RBL that is more parsimonious than its modified counterpart. The proposed method was performed on the simulated as well as the analysis of real data. Sunset yellow and Carmosine as monoprotic acids were determined in candy sample in the presence of unknown interference by this method.