Simultaneous amperometric determination of nickel and copper

A method is described for the amperometric titration of nickel and successive amperometric determination of copper and nickel. Nickel (1.0-16.0 mg) and copper (1.0-11.0 mg) could be determined with an average error of less than 1%. Cobalt interferes but chloride does not. Interference by aluminium, iron(III) and chromium can be eliminated. Zinc and manganese do not interfere if the correct applied voltage is chosen. The procedures can be utilized in the analysis of alloys such as nichrome, Raney nickel, constantan, german silver and manganin. It is best to use the standard addition method for less than 3 mg of nickel.     

Simultaneous determination of creatine and creatinine using amperometric biosensors

In order to determine creatine and creatinine amperometric biosensors were proposed. A bienzymatic biosensor based on creatinase (CI) and sarcosine oxidase (SO) was used for the assay of creatine and a trienzymatic biosensor based on CI, SO and creatininase (CA) for the assay of creatinine. The linear concentration ranges are of pmol l⁻¹ to nmol l⁻¹ magnitude order, with very low limits of detection. The biosensors proved high reliability for determination of creatine and creatinine as raw material, and in the pharmaceutical formulation.     

Conducting organic salt amperometric glucose sensor in continuous-flow monitoring using a wall-jet cell

A simplified method for preparing tetrathiafulvalene?7,7,8,8-tetracyanoquinodimethane-based amperometric enzyme electrodes is described. The electrode is shown to be suitable for the routine monitoring of blood glucose levels. Using the wall-jet cell geometry, the steady-state mode gave more consistent results than the flow-injection mode because of variability in the blood matrix from patient to patient. The results show that, for the wall-jet cell geometry, due consideration must be given to the orientation of the enzyme electrode with respect to the jet inlet. High precision (<2% r.s.d.) and accuracy are then feasible.     

Electrical impedance spectroscopy of gel embedded neuronal cells based on a novel impedimetric biosensor

In this contribution we focus on the on-line analysis of neuronal cells embedded in gel matrices by means of variations in their dielectric and conductive properties. For impedance measurement of thin gel films in flow-through regime a novel impedimetric biosensor was developed. A technique for the preparation of gels containing Neuro-2a neuroblastoma cells (N2a) in between the measurement electrodes was set up. Impedance spectra of gels with N2a cells were analyzed and cell viability was tested. Experimental results showed that even at frequencies (>>1 MHz) and a gel concentration of 2 % with ~8300 cells/μL conductive properties dominate the spectrum.     

Proteome interrogation using nanoprobes to identify targets of a cancer-killing molecule

We report a generic approach for identification of target proteins of therapeutic molecules using nanoprobes. Nanoprobes verify the integrity of nanoparticle-bound ligands in live cells and pull down target proteins from the cellular proteome, providing very important information on drug targets and mechanisms of action. As an example, target proteins as α-tubulin and HSP 90 have been identified and validated.     

Nanoparticle-enhanced sensitivity of a nanogap-interdigitated electrode array impedimetric biosensor

Interdigitated electrode (IDE) arrays with nanometer-scale gaps have been utilized to enhance the sensitivity of affinity-based detection. The geometry of nanogap IDEs was first optimized on the basis of simulations of the electric field and current density. It was determined that the gap (G) between the electrodes was the most important geometric parameter in determining the distribution and strength of the electric field and the current density compared to the width (W) and height (H) of the IDEs. Several devices were materialized and analyzed for their sensitivity to the electrochemical environment using faradic electrochemical impedance spectroscopy (EIS) as the detection technique. Nanogap optimized IDEs were then employed as biosensors for the label-free, affinity-based detection of antitissue transglutaminase antibodies (αtTG-Abs), a biomarker for the detection of autoimmune disorder celiac sprue, triggered by ingesting gluten. The label-free biosensor assay was found to be less sensitive compared to on-chip ELISA. Gold nanoparticles (GNPs) were then employed to improve the sensitivity of the nanogap IDE-based biosensor. With GNPs, the transducer sensitivity increased by 350% over that of label-free detection. The suitability of nanogap IDEs as biosensor transducers for EIS in label-free and GNP-labeled formats was established. The immunobiosensor assay detection sensitivity with the GNPs was found comparable to ELISA.     

An impedimetric assay for the identification of abnormal mitochondrial dynamics in living cells

Mitochondrial dynamics (fission and fusion) plays an important role in cell functions. Disruption in mitochondrial dynamics has been associated with diseases such as neurobiological disorders and cardiovascular diseases. Analysis of mitochondrial fission/fusion has been mostly achieved through direct visualization of the fission/fusion events in live-cell imaging of fluorescently labeled mitochondria. In this study, we demonstrated a label-free, non-invasive Electrical Impedance Spectroscopy (EIS) approach to analyze mitochondrial dynamics in a genetically modified human neuroblastoma SH-SY5Y cell line with no huntingtin protein expression. Huntingtin protein has been shown to regulate mitochondria dynamics. We performed EIS studies on normal SH-SY5Y cells and two independent clones of huntingtin-null cells. The impedance data was used to determine the suspension conductivity and further cytoplasmic conductivity and relate to the abnormal mitochondrial dynamics. For instance, the cytoplasm conductivity value was increased by 11% from huntingtin-null cells to normal cells. Results of this study demonstrated that EIS is sensitive to characterize the abnormal mitochondrial dynamics that can be difficult to quantify by the conventional microscopic method.     

Simultaneous photolysis of directly linked porphyrin-diazonium salt molecule

Meso-tetra-(p-diazoniumphenyl) porphyrin (TDSPP) can be photolyzed only under anaerobic conditions with a yield of 0.18 during simultaneous irradiation with He-Ne laser light (632.8 nm) and light of the 313 nm line of 0 mercury lamp. The excited singlet state of TDSPP is quenched by externalp-methoxybenzene diazoniumtetra fluoroborate (MeODS) with a rate constant of 9.7 × 10⁹M⁻¹s⁻¹. TDSPP and MeODS interact in the ground state with an equilibrium constant of about 16M⁻¹ and form a fluorescent but photochemically inactive.     

Simultaneous achievement of defect passivation and carrier transport promotion by using emerald salt for methylammonium-free perovskite solar cells

Defect passivation along with promoted charge transport is potentially an effective but seldom exploited strategy for high-performance perovskite solar cells (PSCs). Herein, the in situ defect passivation and carrier transport improvement are simultaneously realized by introducing a conductive polymer (i.e., emerald salt, ES) into the precursor solution of methylammonium (MA)-free perovskites. The interaction between ES and uncoordinated Pb²⁺ reduces defect density to suppress the non-radiative recombination. Moreover, ES can act as a “carrier driver” to promote the carrier transport due to its conductive feature, resulting in efficient PSC devices with a decent power conversion efficiency (PCE) of 23.0%, which is among the most efficient MA-free PSCs. The ES-based unencapsulated devices show superior stability, retaining 89.1% and 83.8% of their initial PCEs when subjected to 35 ± 5% relative humidity (RH) storage and 85 °C thermal aging for 1000 h, respectively. To further assess the large-area compatibility of our strategy, 5 × 5 cm² mini modules were also fabricated, delivering an impressive efficiency of 19.3%. This work sheds light on the importance of conductive additives in boosting cell performance by playing multiple roles in passivating defects, retarding the moisture invasion, and enhancing and balancing charge transport.

A conductive polymer, emerald salt (ES), is introduced into methylammonium (MA)-free perovskite solar cells, enhancing the device performance and stability by passivating defects, promoting charge transportation, and retarding the moisture invasion.     

Simultaneous determination of amino acids and carbohydrates by anion-exchange chromatography with integrated pulsed amperometric detection

A direct, sensitive, simple and practical method for simultaneous determination of amino acids and carbohydrates by anion-exchange chromatography with integrated pulsed amperometric detection was developed. The retention behavior of amino acids and carbohydrates on the anion-exchange column and the detection of amino acids and carbohydrates at different integrated pulsed amperometric detection waveforms were investigated. The optimized gradient eluent conditions for analysis of 17 amino acids and nine carbohydrates were obtained. Separation time was 100 min. Detection limits for amino acids and carbohydrates were 5.2-207.1 nM under injection volume of 25 microl. The RSDs of peak area were 1.2-3.3%. The calibration graphs of peak area for the analytes were linear over about three orders of magnitude with a correlation coefficient of 0.9950-0.9999. The method was applied to determine amino acids and carbohydrates in a liquid condiment with satisfactory results.     

Simultaneous determination of electroactive and non-electroactive food preservatives by novel capillary electrophoresis with amperometric detection

A novel capillary electrophoresis and amperometric detection method was achieved by adding an electroactive additive (3,4-dihydroxybenzylamine, 3,4-DHBA) to the running buffer, so that both electroactive and non-electroactive food preservatives were simultaneously determined. Under the selected optimum conditions, four electroactive preservatives (methylparaben, ethylparaben, propylparaben and butylparaben) and two non-electroactive preservatives (potassium sorbate and sodium lactate) were well separated and sensitively detected with detection limits (S/N = 3) ranging from 1.06 × 10⁻⁸ to 2.73 × 10⁻⁶ g mL⁻¹. This method has been successfully employed for the determination of both electroactive and non-electroactive preservatives in several food commodities.     

Simultaneous determination of sulfite and phosphate in wine by means of immobilized enzyme reactions and amperometric detection in a flow-injection system

A flow-injection system is proposed for the simultaneous determination of sulfite and phosphate in wine. A sulfite oxidase immobilized reactor and purine nucleoside phosphorylase-xanthine oxidase co-immobilized reactor are incorporated at fixed positions (parallel configuration) in the flow line, which is based on the splitting of the flow after sample injection and subsequent confluence. A poly(1,2-diaminobenzene)-coated platinum electrode is used as an amperometric detector to detect selectively hydrogen peroxide generated enzymatically in the enzyme reactors, without any interference from oxidizable species and proteins present in wine. Because each channel has a different residence time, two peaks are obtained. The first peak corresponds to sulfite and the second peak to phosphate. The peak current is linearly related to the concentrations of sulfite between 1 × 10⁻⁵ and 2 × 10⁻³M and phosphate between 2 × 10⁻⁵ and 5 × 10⁻³M. The simultaneous determination of sulfite and phosphate in wine can be performed at a rate of 30 samples/hr with satisfactory precision (less than 1.2% RSD) and no pretreatment except for the sample dilution.     

Simultaneous determination of dihydroxybenzene and phenylenediamine positional isomers using capillary zone electrophoresis coupled with amperometric detection

In general capillary zone electrophoresis (CZE) separation models, o‐, m‐, and p‐phenylenediamine isomers can be separated in a weak acidic running buffer for their pK_a values being 4.52, 5.64, 6.04, respectively, while o‐, m‐, and p‐dihydroxybenzene isomers can be separated in a weak basic buffer for their pK_a values being 9.40, 9.40 and 10.04, respectively. So, it is hard to find a suitable running buffer at a fixed pH in normal CZE for simultaneous separation of these two groups of positional isomers. In this paper, a novel method based on alternately running two different pH buffers in CZE coupled with amperometric detection (CZE‐AD) was designed to simultaneously determine these two groups of positional isomers. It is found that when two different pH running buffers were employed alternately under appropriate order and time, the six analytes could be separated perfectly in less than 20 min and the detection limits were as low as 10^–7 mol/L. Furthermore, the effects of working electrode potential, pH and concentration of running buffer, separation voltage and injection time on CZE–AD were investigated. Experimental results demonstrated that the introduced method was practical to simultaneously determine two groups of positional isomers with different pK_a and had some advantages of high sensitivity, good repeatability and small sample requirement.     

Performance of a Faradaic impedimetric immunosensor for blood group antigen A

The performance is described of a label-free Faradaic impedimetric immunosensor based on immobilized monoclonal IgM antibodies to blood group antigen A (anti–A) for blood typing. Anti–A was directly immobilized onto gold electrodes modified with an amine-reactive self assembled monolayer of dithiobis(succinimidylundecanoate). The alteration of the interfacial features of the electrodes due to different modification or recognition steps was probed by Faradaic impedance spectroscopy and cyclic voltammetry in the presence of a hexacyanoferrate(II)/(III) redox couple. Various optimization studies were undertaken with respect to the construction and potential use of the immunosensors as a diagnostic tool for blood typing.     

Development of a functional impedimetric immunosensor for accurate detection of thyroid-stimulating hormone

Thyroid-stimulating hormone (TSH), which regulates the synthesis of thyroid gland hormones affecting the whole metabolism, is a pituitary hormone. Determination of TSH is crucial for monitoring thyroid gland-related disorders and some metabolic diseases.In this study, a nonlabeled immunosensor based on covalent immobilization of anti-TSH antibody by using the formation of self-assembled monolayers (SAM) of 4-mercaptophenylacetic acid (4-MPA) and functionalization of carboxyl ends with 1-ethyl-3-(3-dimetilaminopropil) carbodiimide (EDC)/N-Hydroxysuccinimide (NHS) was fabricated for detection of TSH. Immobilization steps including the concentration of 4-MPA, the concentration of anti-TSH antibody, and duration of anti-TSH antibody incubation were optimized by utilizing electrochemical impedance spectroscopy. Under optimal conditions, a sensitive, rapid, and accurate determination of TSH at a concentration range between 0.7 and 3.5 mIU/L was accomplished with a notable linearity and LOD value of 0.034 mIU/L, as well as reproducibility and repeatability. Moreover, for comparison, linear range experiments were also carried out by using other electrochemical methods, including linear sweep voltammetry, cyclic voltammetry, and capacitance spectroscopy. Finally, the constructed immunosensor was used for analyzing TSH levels spiked in the artificial serum samples.     

Simultaneous amperometric determination of lignin peroxidase and manganese peroxidase activities in compost bioremediation using artificial neural networks

High-performance liquid chromatography (HPLC) and fluorescence derivatization were applied for a nanogram-level N-nitrosodimethylamine (NDMA) analysis of water samples. For the analysis of N-nitrosodimethylamine, samples were first denitrosated by a mixed solution of hydrobromic acid and acetic acid to produce dimethylamine, which was derivatized with dansyl chloride for HPLC fluorescence detection. Fluorescence detection was optimized with excitation and emission wavelengths of 340 and 530 nm, respectively. pH adjustment after denitrosation was necessary to maximize fluorescence intensity with pHs in the range of 9-12. A dansyl chloride concentration of 500 mg l⁻¹ was found to be optimal for measuring a fluorescence signal. An instrumental detection limit of 0.1 ng of NDMA was possible with fluorescence derivatization. The NDMA in water samples was extracted by continuous solid-phase extraction using Ambersorb 572. Although the determination of NDMA was variable at lower concentrations (less than 200 ng l⁻¹), it was observed that the NDMA detection limit with this method could be lowered to a concentration of 10 ng l⁻¹. Another benefit of this method can be found in its selectivity for NDMA. Unlike gas chromatographic (GC) methods, this method generates a distinct peak for NDMA without interference even in the complex matrix of wastewater effluents. The HPLC with fluorescence derivatization method may be applicable for determining NDMA in water and wastewater samples for various research purposes and for screening environmental samples.     

Simultaneous determination of positional isomers of benzenediols by capillary zone electrophoresis with square wave amperometric detection

A capillary zone electrophoresis method coupling square wave amperometric detection (SWAD) for the simultaneous determination of positional isomers of benzendiols (i.e. o-, m-, p-benzenediols) has been developed. Effects of several factors, such as the composition of the running buffer, the pH value, separation voltage, injection time and the potential applied to the working electrode, were investigated to acquire the optimum conditions. The efficacy of the boric acid and ascorbic acid in the running buffer were discussed. o-, m-, p-Benzendiols can be well separated within 8 min in a 50 cm length of 50 microm diameter fused-silica capillary at a separation voltage of +15 kV. Operated in a wall-jet configuration, a 100 microm Pt-disk electrode used as the working electrode exhibits good response for the analytes. The relation between peak current and analyte concentration was linear over two orders of magnitude with detection limits (S/N = 3) ranging from 0.5 to 1.5 microM for all analytes. The proposed method has been successfully applied to monitor the o-, m-, p-benzendiols contents in the environmental wastewater samples with satisfactory assay results.     

Erratum to: Comprehensive interrogation of electrochemical reaction and energy conversion of a direct fucose fuel cell

Journal of Solid State Electrochemistry - In this research, we conducted a comprehensive interrogation of a direct fucose fuel cell to maximise the electric power and demonstrated the potential for...