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    Öğe
    Coordination chemistry of nickel(II), copper(II), and cobalt(II) with MN4 core-containing two novel vic-dioximes ligands.: Synthesis, spectroscopy and redox properties
    (Polish Chemical Soc, 2006) Kilic, A.; Tas, E.; Gumgum, B.; Yilmaz, I.
    Two new vic-dioxime, N-(4-amino-1-benzylpiperidine)-anti-phenylglyoxime(1,1142) and N-(4-amino-1-benzyl piperidine)-anti-glyoxime (L2H2)were prepared by the reaction of anti-phenylchloroglyoxime and anti-monochloroglyoxime with 4-amino1-benzyl piperidine in absolute THF at -15 degrees C. Mononuclear nickel(II), copper(H), and cobalt(H) complexes have a metal-ligand ratio of 1:2 in which the ligands coordinate through the two nitrogen atoms as do most vic-dioximes. The ligands and their Co(II), Cu(II), and Ni(II) complexes were characterized by elemental analyses, FT-IR, UV-vis, H-1-NMR and C-13-NMR, magnetic susceptibility measurements, electrical conductivity measurements and cyclic voltammetry. The electrical conductivity of Ni(II), Co(II), and Cu(II) metal complexes were measured using Four-Point Probe analysis. The electrochemical behavior of the Ni(II), Co(II), and Cu(II) complexes were investigated by cyclic voltammetry in DMSO.
  • [ X ]
    Öğe
    Stability-indicating high performance thin layer chromatographic determination of sulfanilamide in human urine
    (Maik Nauka/Interperiodica/Springer, 2009) Kilinc, E.; Gumgum, B.; Hamamci, C.; Aydin, F.
    A simple, sensitive, selective, precise and stability-indicating high-performance thin-layer chromatographic (HPTLC) method was developed and applied to human urine for the densitometric determination of sulfanilamide. A mixture of chloroform-ethyl acetate-xylene (2.5: 4.0: 1.0, v/v/v) was used as a mobile phase. The system was found to give compact spots for sulfanilamide (retardation factor, R (f) = 0.21 +/- 0.02). The linear regression analysis data for the calibration plots showed good linear relationship with r (2) = 0.9970 +/- 0.0003 and r (2) = 0.9947 +/- 0.020 within the concentration range of 50-250 ng per spot and 100-1000 ng per spot with respect to peak area, respectively. The limit of detection (LOD) and quantification (LOQ) were 8 and 25 ng per spot, respectively. Sulfanilamide was subjected to acid and alkali hydrolysis, oxidation, dry heat and wet heat treatment. According to the International Conference on Harmonization (ICH) guidelines the method was validated for precision, recovery and robustness. The ultraviolet (UV) spectra of the degradation products which had different spectra from sulfanilamide were also recorded.