Abdulkadir Levent

Voltammetric behavior of benzo[a]pyrene at boron-doped diamond electrode: A study of its determination by adsorptive transfer stripping voltammetry based on the enhancement effect of anionic surfactant, sodium dodecylsulfate

Benzo[a]pyrene (BaP), a member of the polycyclic aromatic hydrocarbon (PAH) class, is one of the most potent PAH carcinogens. The electrochemical oxidation of BaP was first studied by cyclic voltammetry at the boron-doped diamond electrode in non-aqueous solvent (dimethylsulphoxide with lithium perchlorate). The compound was irreversibly oxidized in a single step at high positive potential, resulting in the well-resolved formation of a couple with a reduction and re-oxidation wave at much lower potentials. Special attention was given to the use of adsorptive stripping voltammetry together with a medium exchange procedure in aqueous and aqueous/surfactant solutions over the pH range of 2.0-8.0. The technique in aqueous solutions had little value in practice because of too small oxidation peak current. This problem was solved when surfactants were added into the sample solution, by which the oxidation peak currents of BaP were found enhanced dramatically. The employed surfactants were sodium dodecylsulfate (anionic, SDS), cetyltrimethylammonium bromide (cationic, CTAB) and Tween 80 (non-ionic). Using square-wave stripping mode, the compound yielded a well-defined voltammetric response in Britton-Robinson buffer, pH 2.0 containing 2.5×10(-4)M SDS at +1.07 V (vs. Ag/AgCl) (after 120s accumulation at +0.10 V). The process could be used to determine BaP in the concentration range of 16-200 nM (4.04-50.46 ng mL(-1)), with a detection limit of 2.86 nM (0.72 ng mL(-1)). This method was also applied to determine BaP in model water sample prepared by adding its different concentrations into tap water.

Synthesis and Characterization of Cu(II), Co(II), Ni(II), and Zn(II) Complexes of a Schiff Base Derived from 1‐Amino‐5‐benzoyl‐4‐phenyl‐1H‐pyrimidine‐2‐one and 3‐Hydroxysalicylaldehyde

Cu(II), Co(II), Ni(II) and Zn(II) metal complexes of a new heterocylic Schiff base derived from 1‐amino‐5‐benzoyl‐4‐phenyl‐1H‐pyrimidine‐2‐one with 3‐hydroxy‐salicylaldehyde have been synthesized and characterized on the basis of elemental analyses, electronic, IR and 1H NMR spectra, molar conductivity measurements, magnetic moment measurements and thermogravimetric analyses (TGA). It has been found that the Schiff base behaves as a neutral bidentate (NO) or tridentate (ONO) ligand forming chelates with 1:2 (metal:ligand) stoichiometry and octahedral geometry. The conductivity data for the Ni(II) complex is consistent with that expected for a weak electrolyte.

Graphene/Nafion composite film modified glassy carbon electrode for simultaneous determination of paracetamol, aspirin and caffeine in pharmaceutical formulations

A graphene-Nafion composite film was fabricated on the glassy carbon electrode (GR-NF/GCE), and used for simultaneous determination of paracetamol (PAR), aspirin (ASA) and caffeine (CAF). The electrochemical behaviors of PAR, ASA and CAF were investigated by cyclic voltammetry and square-wave adsorptive anodic stripping voltammetry. By using stripping one for simultaneous determination of PAR, ASA and CAF, their electrochemical oxidation peaks appeared at +0.64, 1.04 and 1.44V, and good linear current responses were obtained with the detection limits of 18ngmL(-1) (1.2×10(-9)M), 11.7ngmL(-1) (6.5×10(-8)M) and 7.3ngmL(-1) (3.8×10(-8)M), respectively. Finally, the proposed electrochemical sensor was successfully applied for quantifying PAR, ASA and CAF in commercial tablet formulations.

Synthesis and characterization of 1,2-bis(2-(5-bromo-2-hydroxybenzilidenamino)-4-chlorophenoxy)ethane and its metal complexes: an experimental, theoretical, electrochemical, antioxidant and antibacterial study.

A new Schiff base ligand was synthesized by reaction of 5-bromosalicylaldehyde with 1,2-bis(4-chloro-2-aminophenoxy)ethane. Then the Schiff base complexes were synthesized by the reaction of metal salts and the novel Schiff base. The molar conductivity properties of the complexes were studied and found out that the complexes are nonelectrolytes. The structures of the ligand and its metal complexes were characterized by elemental analysis, FT-IR, UV-VIS, magnetic susceptibility measurements, molar conductivity measurements, and thermal gravimetric analysis. In addition antioxidant, theoretical NMR studies and cyclic voltammetry of the complexes were done. Two methods namely metal chelating activity and diphenylpicrylhydrazyl (DPPH) radical scavenging method were used to determine the antioxidant activity, and antibacterial properties of the compounds were also studied.

Synthesis, characterization and experimental, theoretical, electrochemical, antioxidant and antibacterial study of a new Schiff base and its complexes

A new Schiff base ligand was synthesized by reaction of salicylaldehyde with 1,6-bis(4-chloro-2-aminophenoxy)hexane. Then the Schiff base complexes were synthesized by metal salts and the Schiff base. The metal to ligand ratio of metal complexes was found to be 1:1. The Cu(II) complex is proposed to be square planar and the Co(II), Ni(II), Mn(II) and Zn(II) complexes are proposed to be tetrahedral geometry. The Ti(III) and V(III) complexes are proposed to be a capped octahedron in which a seventh ligand has been added to triangular face. The complexes are non-electrolytes as shown by their molar conductivities (ΛM). The structure of metal complexes is proposed from elemental analysis, FT-IR, UV-vis, magnetic susceptibility measurements, molar conductivity measurements, Mass Spectra and thermal gravimetric analysis. In addition antimicrobial and antioxidant studies, cyclic voltammetry of the complexes, theoretical 1H NMR and HOMO-LUMO energy calculations of the new di-functional ligand were done.

Electrooxidation of thiourea and its square-wave voltammetric determination using pencil graphite electrode

Abstract The electrochemical properties of thiourea (TU) were investigated in pH range 2.0–12.0 by cyclic and square-wave voltammetry. The compound was irreversibly oxidized at a pencil graphite electrode in one or two oxidation steps which are pH-dependent. Based on the voltammetric peak for the second oxidation process of TU in phosphate buffer at pH 12.0, a square-wave voltammetric method was proposed for the determination of the compound in the range 6.3–30μm, with a detection limit of 1.29μm. The applicability to direct assays of wastewaters was also tested.

Colorimetric and Atomic Absorption Spectrometric Determination of Mucolytic Drug Ambroxol Through Ion-Pair Formation with Iron and Thiocyanate

Colorimetric and atomic absorption spectrometric methods have been developed for the determination of mucolytic drug Ambroxol. These procedures depend upon the reaction of iron(III) metal ion with the drug in the presence of thiocyanate ion to form stable ion-pair complex which extractable chloroform. The red-coloured complex was determined either colorimetrically at 510 nm or by indirect atomic absorption spectrometry (AAS) via the determination of the iron content in the formed complex. The optimum experimental conditions for pH, concentrations of Fe(3+) and SCN(-), shaking time, phase ratio, and the number of extractions were determined. Under the proposed conditions, linearity was obeyed in the concentration ranges 4.1x10(-6) - 5.7x10(-5) M (1.7-23.6 µg mL(-1)) using both methods, with detection limits of 4.6x10(-7) M (0.19 µg mL(-1)) for colorimetry and 1.1x10(-6) M (0.46 µg mL(-1)) for AAS. The proposed methods were applied for the determination of Ambroxol in tablet dosage forms. The results obtained were statistically analyzed and compared with those obtained by applying the high-performance liquid chromatographic method with diode-array detection.

The effect of Plantago major Linnaeus on serum total sialic acid, lipid-bound sialic acid, some trace elements and minerals after administration of 7,12-dimethylbenz(a)anthracene in rats.

The present study was designed to evaluate the effect of Plantago major Linnaeus (PM) extract on serum total sialic acid (TSA), lipid-bound sialic acid (LSA), some trace elements (copper (Cu), zinc (Zn) and iron) and mineral levels (magnesium, calcium and sodium) in Wistar albino rat administrated 7,12-dimethylbenz(a)anthracene (DMBA). Rats were divided into three equal groups (n = 6). Group I comprised the control group, group II was treated with DMBA (100 mg/kg, single dose) and group III was treated with DMBA (100 mg/kg single dose) and aqueous extract of PM 100 mg/kg/day for 60 days. After 60 days, statistical analyses showed that TSA and LSA levels in DMBA and DMBA + PM groups were significantly higher compared to the control group (TSA: p < 0.01, p < 0.05; LSA: p < 0.05, p < 0.05, respectively). Serum Zn levels were decreased in subjects treated with DMBA (p < 0.01) and DMBA + PM (p < 0.05) compared to the control group values. Serum Cu levels were increased in DMBA group and PM-treated group compared to the control group values. The results of this investigation showed that the levels of TSA and LSA changed significantly, which are sensitive markers for detecting the toxic effects of DMBA. On the other hand, observed decline in Zn levels in rats from DMBA + PM group might be due to decreased generation of free radicals and oxidative stress. Results from this study suggest that PM may be partially effective in preventing carcinogenesis initiated by environmental carcinogen DMBA.

Synthesis and Characterization of a New Difunctional Ligand and Its Metal Complexes: An Experimental, Theoretical, Cyclic Voltammetric, and Antimicrobial Study

A new difunctional Schiff base ligand and its some metal complexes were synthesized. The compounds were characterized by elemental analysis, 1H-NMR, 13C-NMR, FT-IR, UV-VIS, magnetic susceptibility measurements, molar conductivity measurements, and thermal gravimetric analysis techniques. Additionally, DPPH scavenging, metal chelating and antibacterial activity of compounds were examined via in vitro methods. The lowest DPPH scavenging activity observed by Co(II) as 36.28% and highest was ligand as 52.00%. A cyclic voltammetric study was also carried out to determine redox potentials of the compounds. Some theoretical studies such as 1H-NMR, HOMO-LUMO, and mapped electron density of the ligand were also carried out successfully.

Determination of 7,12-dimethylbenz[a]anthracene in orally treated rats by high-performance liquid chromatography and transfer stripping voltammetry.

A number of polycyclic aromatic hydrocarbons (PAHs) have been shown to be toxicants, and induce carcinogenic and immunotoxic effects. As a model PAH agent, 7,12-dimethylbenz[a]anthracene (DMBA) was the strongest one tested in terms of its biological activities and biotransformation. A new and simple high-performance liquid chromatographic (HPLC) method with diode-array detection at 290 nm was developed and validated for monitoring of DMBA in different matrices (serum, liver and kidney) of rats orally treated with DMBA. Furthermore, the applicability of adsorptive transfer stripping voltammetry (AdTSV) on the pencil-lead graphite electrode to these samples was illustrated using our previously reported data for bulk aqueous solutions of DMBA. HPLC and AdTSV methods, which were compatible with each other, allowed DMBA to be detected down to the levels of 3.82x10-9 M (0.98 ppb) and 6.73x10-9 M (1.73 ppb), respectively. Olive oil solutions of DMBA in dose 50 mg/kg were orally administered. 60 days after a single dose of DMBA, its concentrations in these biological samples from rats were measured by means of both methods. Because of rapid biotransformation, DMBA could not be detected in serum. Only low levels of the compounds were deposited unchanged in kidney whereas its levels were considerably higher in liver. These methods were also applied to the assay whether there is an influence of the intake of aqueous extracts of Hypericum Perforatum L. plant on the parent DMBA levels accumulated in rat tissues.