Evaluation of the antioxidant activity by flow injection analysis method with electrochemically generated ABTS radical cation

A Trolox equivalent antioxidant capacity (TEAC) decolourisation assay was adapted to a flow injection analysis (FIA) system and a simple and rapid method for antioxidant activity evaluation was developed. To avoid the time consuming step of 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid)(ABTS) radical cation preparation by chemical oxidation of ABTS, as in the original TAEC assay, and hence, to shorten the analysis time, the ABTS radical cation was generated on-line by electrochemical oxidation of ABTS in the flow-through electrolysis cell forming a part of the FIA system. The proposed method was optimised with respect to a flow rate, injection volume and ABTS radical cation/carrier ratio. Under the optimised conditions linear calibration graphs for Trolox were obtained over the range 10-100 microM, with a limit of detection 1.6 microM. Good reproducibility (relative standard deviation 1.95%) and sample throughput (32 samples per hour) were achieved. The developed method was applied to the evaluation of the antioxidant activity of pure compounds and samples of some common beverages. In both cases a good correlation between the results obtained by the proposed method and TEAC values evaluated by the classic TAEC decolourisation assay was obtained (r(2)= 0.996 for pure compounds and r(2)= 0.957 for beverage samples).     

On the Integrability of Geodesic Flows of Submersion Metrics

Letters in Mathematical Physics - Suppose we are given a compact Riemannian manifold (Q,g) with a completely integrable geodesic flow. Let G be a compact connected Lie group acting freely on Q by...     

Antimony Film Microelectrode for Anodic Stripping Measurement of Cadmium(II), Lead(II) and Copper(II)

The antimony film microelectrode (SbFME) is presented for measuring trace heavy metal ions in combination with anodic stripping voltammetry. The SbFME was tested in model solutions of 0.01 M HCl containing Cd(II) and Pb(II) in the presence of dissolved oxygen. The microsensor exhibited good linear behavior in the examined concentration range 20 μg L⁻¹ to 100 μg L⁻¹ and LoD of 1.9 and 3.1 μg L⁻¹ for Cd(II) and Pb(II), respectively. The suitability of SbFME for measuring trace levels of Cu(II) was demonstrated using the standard reference material of natural water exploiting the sensor's specific characteristic of low re‐oxidation signal for antimony.     

Bismuth film electrode for anodic stripping voltammetric determination of tin

The bismuth film electrode (BiFE), in combination with anodic stripping voltammetry, offers convenient measurement of low concentrations of tin. The procedure involves simultaneous in situ formation of the bismuth film electrode on a glassy carbon substrate electrode, together with electrochemical deposition of tin, in a non-deaerated model solution containing bismuth ions, catechol as complexing agent and the metal analyte, followed by an anodic stripping scan. The BiFE is characterized by an attractive electroanalytical performance, with two distinct voltammetric stripping signals corresponding to tin, accompanied with low background contributions. Several experimental parameters were optimized, such as concentration of bismuth ions and catechol, deposition potential, deposition time and pH of the model solution. In addition, a critical comparison is given with bare glassy carbon and mercury film electrodes, revealing the superior characteristics of BiFE for measurement of tin. BiFE exhibited highly linear behavior in the examined concentration range from 1 to 100 μg L⁻¹ of tin (R² = 0.997), an LoD of 0.26 μg L⁻¹ tin, and good reproducibility with a calculated R.S.D. of 7.3% for 10 μg L⁻¹ tin (n = 10). As an example, the practical applicability of BiFE was tested with the measurement of tin in a real sample of seawater.     

Perspectives of carbon paste electrodes in stripping potentiometry.

The testing of various types of carbon paste electrodes (CPEs) for their use in stripping potentiometry was carried out by means of specially proposed procedures and by using various model analyte systems. CPEs containing three different pasting liquids (paraffin oil, silicone oil, tricresyl phosphate) were tested as supports for mercury- and gold films, and as substrates for electrolytic, adsorptive, ion-pair forming, and extractive accumulation. Test measurements in organic solvent-containing media and studies of some irreversible electrochemical reactions were performed as well. Individual examples to be studied allowed one to formulate and outline some perspectives of CPEs in potentiometric stripping analysis and related constant current stripping analysis.     

Ex Situ Prepared Antimony Film Electrode for Electrochemical Stripping Measurement of Heavy Metal Ions

The antimony film electrode (SbFE) was prepared ex situ for anodic and adsorptive stripping voltammetric measurement of selected heavy metal ions. The electrode revealed good linearity for Cd(II) and Pb(II) in a nondeaerated solution of 0.01 M HCl in the examined concentration range from 25 to 80 μg L^?1 with limits of detection of 1.1 μg L^?1 for Cd(II) and 0.3 μg L^?1 for Pb(II) and an excellent reproducibility. The preplated SbFE was also preliminary tested for measuring low levels of Ni(II) using adsorptive stripping voltammetry exhibiting good linearity and sensitivity in combination with only a 30 s deposition step.     

A novel amperometric method for antioxidant activity determination using DPPH free radical

A new method for the determination of antioxidant activity based on the amperometric reduction of 2,2-diphenyl-1-picrylhydrazyl (DPPH) at the glassy carbon electrode is proposed. All experiments were done in three-electrode electrochemical cell at 140 mV vs. Hg(2)Cl(2) | 3 M KCl using ethanolic solution (phi=40%) and 0.033 M KCl in 0.033 M phosphate buffer, pH=7.4. The linear range obtained for Trolox in 100 microM DPPH ethanol-water solution was up to 30 microM, with a limit of detection of 0.05 microM. The developed method was applied for the evaluation of antioxidant activity of some water or ethanol soluble pure compounds of antioxidants and of the samples of tea, wine and some other beverages. The good correlation of measurements (R(2)=0.9993) expressed as Trolox equivalent was obtained between the proposed amperometric method and classic spectroscopic method.     

Mössbauer effect and first principle calculations of the electronic structure and hyperfine interaction parameters of Hf2Fe

A detailed theoretical study of the structure, electronic properties and the electric field gradients of the Hf₂Fe intermetallic compound is presented. Using all-electron full-potential linearized augmented plane wave (FP-LAPW) formalism the equilibrium volume, bulk modulus and electric field gradients are calculated. The obtained results are compared with EFG values inferred from measurements performed using Mössbauer spectroscopy and the earlier reported time differential perturbed angular correlation (TDPAC) measurements. The lattice relaxation and the supercell calculations are found to be essential for the correct interpretation of the experimental results.     

Response Behavior of Amperometric Glucose Biosensors Based on Different Carbon Substrate Transducers Coated with Enzyme‐Active Layer: A Comparative Study

Carbon electrodes (glassy carbon, GC, screen‐printed carbon, SPC, and carbon fiber, CF) were used as substrate transducers to prepare glucose biosensors of different sizes and geometries, based on iron‐ruthenium hexacyanoferrate as H₂O₂ reduction mediator and glucose oxidase immobilized in a poly(1,2‐phenylenediamine) membrane. Their response behavior under hydrodynamic amperometric conditions at an operating potential of ?0.02 V vs. Ag/AgCl was studied and compared. While the GC and SPC based conventional size biosensors showed enzymatic catalysis controlled current response with nonlinear concentration dependence, the CF based micro‐biosensor exhibited, due to diffusion‐controlled current response, extended linear range calibration curves with relatively lower sensitivity and longer response times. Several preparation parameters responsible for the improvement of biosensor performance were also investigated.