Trimethoprim drug (TMP) complexes of copper (II), cobalt (II), and nickel (II) were prepared and discussed by using elemental analysis (C, H, N analysis), magnetic, molar conductance, FTIR, Raman spectroscopy, electron spin resonance (ESR) and UV-vis spectroscopy analyses. TMP drug coordinated as a tridentate ligand towards the respected three metal ions through two nitrogen atoms of amino groups and nitrogen atom of pyrimidine ring which flanked between –NH2 groups, these assignments confirmed by spectroscopic, magnetic, ESR and thermogravimetric analyses with formulas [Cu(TMP)(H2O)3]Cl2, [Co(TMP)(H2O)3]Cl2 and [Ni(TMP) (H2O)]Cl2. Copper (II) and cobalt (II) complexes have an octahedral geometrical structure included one TMP molecule, three coordinated water molecules and two uncoordinated chlorine atoms while, nickel(II)–TMP complex has a tetrahedral geometric configuration that involved one TMP molecule, one coordinated water molecule and two uncoordinated chlorine atoms. The activation energies and other kinetic thermodynamic parameters were estimated based on the employed of the Coats-Redfern and Horowitz-Metzger equations. The nano–structured form of the synthesized TMP complexes was confirmed dependent on the transmission electron microscopy (TEM).
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An adsorptive stripping voltammetric procedure for the determination of trimethoprim at an in situ plated lead film electrode on glassy carbon substrate was described. The lead film plating process and accumulation of trimethoprim were performed simultaneously in an acetate buffer solution of pH = 5.8 and at potential -1.275 V. The measurements were carried out in undeaerated solutions. The calibration graph, for an accumulation time of 60 s, was linear in the range from 1 x 10-8 to 2x10-7 mol L-1. The detection limit was 3.5 x 10-9 mol L-1: the relative standard deviation for 1 x 10-7 mol L-1 trimethoprim was 4.2%. The proposed procedure was successfully applied to trimethoprim determination in pharmaceutical preparations and human urine samples.
PL
W pracy opisano procedurę oznaczania trimetoprimu na tworzonej in situ błonkowej elektrodzie ołowiowej na podłożu z węgla szklistego, metodą adsorpcyjnej woltamperometrii stripingowej. Tworzenie bionki ołowiu i zateżanie trimetoprimu przeprowadzano jednocześnie, z roztworu buforu octanowego o pH = 5,8, przy potencjale -1.275 V. Pomiary wykonywano z roztworów nieodtlenionych. Krzywa kalibracyjna przy czasie zatężania 60 s jest liniowawzakresieod l x 10-8 do 2x 10-7 mol L-1. Granica wykrywalności wynosi 3.5 x 10-9 mol L-1 a względne odchylenie standardowe, przy oznaczaniu trimetoprimu o stężeniu l x 10-7 mol L-1 wynosi 4,2%. Zaprezentowana procedura została wykorzystanado oznaczania trimetoprimu w preparatach farmaceutycznych i próbkach ludzkiego moczu.
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