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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 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.
