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Öğe Design, preparation and application of a Pirkle-type chiral stationary phase for enantioseparation of some racemic organic acids and molecular dynamics studies(ACG Publications, 2017-11) Çakmak, Reşit; Ercan, Selami; Sünkür, Murat; Yılmaz, Hayrullah; Topal, GirayThis study consists of two parts. In the first part of the study; a Pirkle-type chiral stationary phase was prepared by synthesizing an aromatic amine derivative of (R)-2-amino-1-butanol as a chiral selector and binding to L-tyrosine-modified cyanogen bromide (CNBr)-activated Sepharose 4B and then, packed into the separation column. The chromatographic performance of the separation column was evaluated with racemic mandelic acid and 2-phenylpropionic acid by using phosphate buffers at three different pHs as mobile phase. In the resolution processes, the prepared solutions were loaded onto the separation column at two different concentrations and at three different pHs for each racemic organic acid, separately. Enantiomeric excess (ee%) of the eluates was determined on CHIRALPAK AD-H chiral analytical column by HPLC. The maximum ee% for mandelic acid and 2-phenylpropionic acid was determined to be 60.84 and 27.4, respectively. Separation factors (k1 ’ , k2 ’ , α, and Rs) were calculated for each acid. The structures of the obtained compounds were characterized using the spectroscopic methods (NMR, and elemental analysis). In the second part of the study; enantioselective interactions between the prepared CSP and the analytes have been widely studied by docking, molecular dynamics simulation and quantum mechanical computation methods. The reason of column eluation of rac-2-phenylpropionic acid with lower enantiomeric yield was explained by these techniques.Öğe Synthesis and anticorrosion studies of 4-[(2-nitroacetophenonylidene)-amino]-antipyrine on SAE 1012 carbon steel in 15 wt.% HCl solution(Taylor & Francis, 2020-11-16) Gerengi, Hüsnü; Çakmak, Reşit; Dağ, Beşir; Solomon, M. M; Tüysüz Akbal, Hatice Aslıhan; Kaya, ErtuğrulA novel corrosion inhibitor, ((E)-1,5-dimethyl-4-((1-(3-nitrophenyl)ethylidene)amino)-2-phenyl-1,2-dihydro-3H-pyrazol-3-one) (DNPP) was synthesized in high yield by the condensation reaction of 4-aminoantipyrine with 2-nitroacetphenone derived from acetophenone as a starting material and characterized by FT-IR, 1H, and 13C NMR techniques. DNPP was tested against the corrosion of SAE 1012 carbon steel in 15 wt.% HCl solution using electrochemical and surface characterization techniques. Results obtained show that DNPP is effective in retarding the corrosion of SAE 1012 carbon steel. With 4 mM of DNPP, the charge transfer resistance of SAE 1012 in 15 wt.% HCl solution is raised from 17.42 to 140.50 Ω cm2 and the substrate surface is protected by 87%. The inhibition is through adsorption mechanism (mixed-adsorption type) and has been confirmed by SEM and EDAX results. Potentiodynamic polarization results reveal that DNPP acted as a mixed-type corrosion inhibitor. DNPP is a promising candidate for the formulation of an inhibitor cocktail for the strong acid environment.Öğe Simultaneous electrochemical evaluation of ascorbic acid, epinephrine and uric acid at disposable pencil graphite electrode: Highly sensitive determination in pharmaceuticals and biological liquids by differential pulse voltammetry(Elsevier, 2018) Levent, Abdulkadir; Önal, GünayAim and Objective: As is known, AA, EP and UA can also coexist in biological fluids. Therefore, the determination of the levels of these compounds in biological fluids is extremely important both for the diagnosis and treatment of the related diseases. In the presence of many interfering substances in biological fluids such as blood and urine samples, it is very important that these compounds can be selectively analyzed. Materials and Methods: All electrochemical experiments were performed using an Autolab PGSTAT 128N potentiostat. Before beginning the electrochemical measurements, the PGE was activated. The electrochemical pretreatment of PG was exercised by anodically +1.40 V for 60 s. Then, measurements were performed with CV (-0.4 V to 1.2 V) and DPV (-0.2 V to 0.7 V) for single and simultaneous voltammetric behaviour of AA, EP, and UA in the electrochemical method. Results: The anodic peak potentials of AA and UA were observed at about +0.32 V and +0.62 V, respectively. On the other hand, for EP, while anodic peak potential was observed at about +0.53 V, in the reverse scan, cathodic peak potentials were observed at about +0.41 V and +0.007 V. The39 reduction peak observed at +0.3 V with the oxidation peak observed at +0.53 V are the reversible peaks. In the method developed for the electrochemical simultaneous determination of AA, EP and UA using PGE with DPV technique in BR buffer solution (pH 4.0), the anodic peak potentials are sufficiently separated from each other. Conclusion: A voltammetric method was developed for the simultaneous determination of AA, EP and UA with PGE for the first time. Here, the most important thing is that the simultaneous determination of AA, EP and UA was successfully achieved with that targeted voltammetric method which was sensitive, low-cost, practical and well-repeated; and that these were proven to be selectively applicable in pharmaceutical products and biological liquids.Öğe Application of a pencil graphite electrode for voltammetric simultaneous determination of ascorbic acid, norepinephrine, and uric acid in real samples(TÜBİTAK, 2018-04-27) Levent, Abdulkadir; Önal, GünayA pencil graphite electrode (PGE) was used for the simultaneous detection of ascorbic acid (AA), norepinephrine (NE), and uric acid (UA) by differential pulse voltammetry and cyclic voltammetry. The anodic peaks of AA, NE, and UA in their mixture can be well separated in 0.1 M Britton–Robinson buffer solution at pH 4.0. The effects of various experimental parameters such as pH, scan rate, and voltammetric parameters on the voltammetric response of these compounds were investigated. Under optimum conditions, linear calibration graphs were obtained from the AA, NE, and UA concentration ranges, which were 100–800 nM, 20–170 nM, and 40–175 nM, respectively. The detection limits for AA, NE, and UA were 27 nM, 4 nM, and 10 nM in the form of a mixture at the PGE. This electrode shows great analytical performance characteristics, corresponding repeatability and recovery for the simultaneous determination of these compounds. PGE, which was used for the first time in this method, has been successfully applied for the assay of UA in human urine samples with the aim of determining AA and NE in pharmaceutical drugs.
