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Öğe Benzoil ester grubu içeren 2,4-dinitrofenilhidrazin temelli bazı yeni hidrazon bileşiklerinin sentezi ve yapısal karakterizasyonu(Batman Üniversitesi, 2022-06-30) Çakmak, Reşit; Başaran, EyüpHidrazon bileşikleri, ilaç tasarımı çalışmalarında aday bileşikleri elde etmek için kullanılan önemli öncülerdir. Bu çalışmada, başlangıç materyali olarak 4-(dietilamino) salisilaldehitten türetilen benzoil ester türevleri (1-5) sübstitüe benzoil klorür türevleri (benzoil klorür, 2-nitrobenzoil klorür, 3-nitrobenzoil klorür, 4-nitrobenzoil klorür ve 3,5-dinitrobenzoil klorür) ile çözücü olarak piridin ortamında 1:1 mol oranında reaksiyona girmesiyle sentezlendi. Elde edilen benzoil esterler ile 2,4-dinitrofenilhidrazinin kondenzasyon reaksiyonu ile yeni bir dizi hidrazon bileşikleri (6-10) sentezlendi ve bu bileşikler yapısal karakterizasyonu FT-IR, 1H NMR, 13C NMR ve element analizi aydınlatıldı. Sonuç olarak, bu bileşiklerin biyolojik aktiviteler gösterebileceği düşünülmektedir.Öğe Silica gel-immobilized 5-aminoisophthalohydrazide: A novel sorbent for solid phase extraction of Cu, Zn and Pb from natural water samples(Wiley Online Library, 2020-03-11) Aydın, Funda; Çakmak, Reşit; Levent, Abdulkadir; Soylak, MustafaA novel silica sorbent, silica gel‐immobilized 5‐aminoisophthalohydrazide (SiO2‐APH), was prepared by the condensation of 3‐chloropropyl‐functionalized silica gel with 5‐aminoisophthalohydrazide (APH) derived from dimethyl 5‐aminoisophthalate as a starting material and used for separation and preconcentration of Cu, Zn, and Pb metals in water samples using Flame Atomic Absorption Spectrometry (FAAS). The characterization of the new sorbent was carried out by Elemental Analysis, Thermogravimetric Analysis (TGA) and Fourier Transform Infrared Spectroscopy (FTIR). Important analytical parameters including as pH, amount of sorbent, type and amount of eluting solvent, sample volume, vortex and ultrasonic bath time, matrix ions that effect the developed SiO2‐APH‐solid phase extraction (SPE) method were investigated and optimum parameters were detected. Recoveries of examined metals were obtained as 98% for Cu and Pb and 101% for Zn. The relative standard deviation (RSD, n = 8) of Cu, Zn and Pb metals were 3.2, 2.8 and 1.6%, respectively. Limit of detections (LODs) (n = 10) were found as 2.7 μg L−1 for Cu, 7.4 μg L−1 for Zn and 3.5 μg L−1 for Pb μg L−1. The accuracy of the new method was assessed by analyzing of TMDA‐51.4 and TMDA‐70.2 certified reference materials. The results obtained for metals were in a good agreement with certified values. Addition/recovery test was applied to the real well, river, dam and stream water samples to check the accuracy of the method. The results showed that the developed SiO2‐APH‐SPE method can be effectively used as an alternative method for determination of Cu, Zn, and Pb metals in water samples.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.
