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Öğe Fluorescence properties and electrochemical behavior of some schiff bases derived from n-aminopyrimidine(Springer Nature, 2014-03) Gülcan, Mehmet; Doğrul, Ümit; Öztürk Ürüt, Gülsiye; Levent, Abdulkadir; Akbaş, EsvetA series of Schiff bases (L 1, L 2 and L 3 ) were prepared by refluxing aromatic aldehydes with N-Aminopyrimidine derivatives in methanol and ethanol. The structures of synthesized compounds were characterized by FTIR, 1H NMR, 13C NMR and microanalysis. The electrochemical behaviors of the Schiff base ligands were also discussed. Moreover, the evaluation of absorption and emission properties of the structures were carried out in five different solvents. The products show visible absorption maxima in the range of 304-576 nm, and emission maxima from 636 to 736 nm in all solvents tested.Öğe Synthesis, characterization and application of a novel multifunctional stationary phase for hydrophilic interaction/reversed phase mixed-mode chromatography(Talanta, 2017-11-1) Aral, Tarık; Aral, Hayriye; Çelik, Kadir Serdar; Altındağ, RamazanA novel multifunctional stationary phase based on silica gel was synthesised starting from L- isoleucine and 4-phenylbutylamine and evaluated as a hydrophilic interaction/reversed-phase mixed-mode stationary phase for high-performance liquid chromatography (HPLC). The prepared stationary phase was characterized by elemental analysis, infrared spectroscopy (IR), scanning electron microscopy (SEM), Brunauer, Emmett and Teller (BET) and solid-state 13C nuclear magnetic resonance (NMR). The mechanisms involved in the chromatographic separation are multi-interaction, including hydrophobic, π-π, hydrogen-bonding, dipole-dipole and ion-dipole interactions. Based on these interactions, successful separation could be achieved among several aromatic compounds having different polarities under both hydrophilic interaction liquid chromatography (HILIC) and reversed phase (RP) condition. Nucleotides/nucleosides were separated in the HILIC mode. The effects of different separation conditions, such as pH value, mobile-phase content, column temperature, buffer concentration and flow rate, on the separation of nucleotides/nucleosides in HILIC mode were investigated. The seven nucleotides/nucleosides were separated within 22 min, while six of them were separated within 10 min by isocratic elution. To determine the influence of the new multifunctional stationary phase under the RP condition, a number of moderately and weakly polar and nonpolar compounds, such as 10 substituted anilines and eight substituted phenols were separated successfully under the RP condition within 14 and 15 min, respectively. Additionally, nine mixtures of polar/nonpolar test compounds were simultaneously separated within 19 min, while seven of them were separated within 12 min, under HILIC/RP mixed-mode conditions. Chromatographic parameters, such as the retention factor and peak asymmetry factor, were calculated for all of the analytes, while the theoretical plate number was calculated for analytes separated by isocratic elution. Compared to traditional C18 and commercial HILIC columns, the new stationary phase exhibited both HILIC and RPLC performance, and the scope of analyte separation was thus enlarged.Öğe Magnetite nanoparticles grafted with murexide-terminated polyamidoamine dendrimers for removal of lead (II) from aqueous solution: synthesis, characterization, adsorption and antimicrobial activity studies(Journals & Books, 2021-03) Ekinci, Selma; İlter, Zülfiye; Ercan, Selami; Çınar, Ercan; Çakmak, ReşitIn this study, new, efficient, eco-friendly and magnetically separable nanoadsorbents, MNPs-G1-Mu and MNPs-G2-Mu, were successfully prepared by covalently grafting murexide-terminated polyamidoamine dendrimers on 3-aminopropyl functionalized silica-coated magnetite nanoparticles, and used for rapid removal of lead (II) from aqueous medium. After each adsorption process, the supernatant was successfully acquired from reaction mixture by the magnetic separation, and then analyzed by employing ICP-OES. Chemical and physical characterizations of new nanomaterials were confirmed by XRD, FT-IR, SEM, TEM, and VSM. Maximum adsorption capacities (qm) of both prepared new nanostructured adsorbents were compared with each other and also with some other adsorbents. The kinetic data were appraised by using pseudo-first-order and pseudo-second-order kinetic models. Adsorption isotherms were found to be suitable with both Langmuir and Freundlich isotherm linear equations. The maximum adsorption capacities for MNPs-G1-Mu and MNPs-G2-Mu were calculated as 208.33 mg g−1 and 232.56 mg g−1, respectively. Antimicrobial activities of nanoparticles were also examined against various microorganisms by using microdilution method. It was determined that MNPs-G1-Mu, MNPs-G2-Mu and lead (II) adsorbed MNPs-G2-Mu showed good antimicrobial activity against S. aureus ATTC 29213 and C. Parapsilosis ATTC 22019. MNPs-G1-Mu also showed antimicrobial activity against C. albicans ATTC 10231.Öğe Electrochemical performance of boron-doped diamond electrode in surfactant-containing media for ambroxol determination(Elsevier, 2014-07-17) Levent, Abdulkadir; Yardım, Yavuz; Şentürk, ZühreA novel application of boron-doped diamond electrode is introduced for the determination of ambroxol, a potential antioxidant drug belonging to the expectorant class. The electrochemical oxidation of ambroxol was first investigated by cyclic voltammetry using boron-doped diamond and glassy carbon electrodes in aqueous solutions both with and without the addition of surfactant. The compound was irreversibly oxidized in one/two steps at high positive potentials, resulting in the formation of a couple with a reduction and re-oxidation wave at less positive potentials. Special attention was given to the use of adsorptive stripping voltammetry at a surface of mildly oxidized boron-doped diamond electrode in aqueous solutions over the pH range of 1.0–10.0. Addition of anionic surfactant (sodium dodecylsulfate) to ambroxol-containing electrolyte enhanced the stripping current signal. Using square-wave stripping mode, the drug yielded a well-defined voltammetric response in phosphate buffer pH 2.5 containing 4 × 10−4 M sodium dodecylsulfate at +1.02 V (versus Ag/AgCl) (after 30 s accumulation at +0.50 V). The process could be used to determine ambroxol in the concentration range of 0.05–0.7 μM, with a detection limit of 0.010 μM (4.2 ng mL−1). The suggested method was successfully applied to pharmaceuticals and spiked human urine samples.Öğe Preparation of a novel ionic hybrid stationary phase by non-covalent functionalization of single-walled carbon nanotubes with amino-derivatized silica gel for fast HPLC separation of aromatic compounds(Elsevier, 2016-03) Aral, Hayriye; Çelik, Kadir Serdar; Aral, Tarık; Topal, GiraySingle-walled carbon nanotubes (SWCNTs) were immobilized on spherical silica gel with a 4-μm average particle size and a 60-Å average pore size. The amino-derivatized silica gel was non-covalently coated with carboxylated SWCNTs to preserve the structure of the nanotubes and their physico-chemical properties. The novel ionic hybrid stationary phase was characterized by scanning electron microscopy (SEM), infra-red (IR) spectroscopy and elemental analysis, and then, it was used to fill an empty 150×4.6 mm 2 high-performance liquid chromatography (HPLC) column. Chromatographic parameters, such as the theoretical plate number, retention factor and peak asymmetry factor, and analytical parameters, such as the limit of detection (LOD), limit of quantification (LOQ), linear range, calibration equation, and R 2 value, and quantitative analysis parameters were calculated for all of the analytes. Using different mobile phases, five different classes of aromatic hydrocarbons were separated in a very short analysis time of 4-8 min. Furthermore, a high theoretical plate number (up to 25000) and an excellent peak asymmetry factor (1.0) were obtained. The results showed that the surface of the SWNTs had very strong interactions with aromatic groups, therefore providing high selectivity for the separation of different classes of aromatic compounds. This study indicates that SWCNTs enable the extension of the application range of the newly prepared stationary phases for the fast separation of aromatic compounds by HPLC.Öğe Novel C2-symmetric macrocycles bearing diamide-diester groups: Synthesis and enantiomeric recognition for primary alkyl ammonium salts(American Chemical Society, 2008-03-12) Sünkür, Murat; Barış Cebe, Deniz; Hoşgören, Halil; Toğrul, MahmutWe synthesized a series of novel macrocycles with diamide−diester groups (S,S)-1, (S,S)-2, (S,S)-3, and (R,R)-1, derived from dimethyloxalate and amino alcohols by high dilution technique, and evaluated enantiomeric recognition properties of these macrocycles toward primary alkyl ammonium salts by 1H NMR titration. Taking into account the host employed, important differences were observed in the Ka values of (R)-Am and (S)-Am for (S,S)-1 and (R,R)-1 hosts, KS/KR = 5.55 and KR/KS = 3.65, ΔΔGo = 0.43 and −0.32 kJ mol-1, respectively. There seems a general tendency for the host to include the guests with the same absolute configuration.Öğe Synthesis, characterization, and application of a novel multifunctional stationary phase for hydrophilic interaction/reversed phase mixed-mode chromatography(Elsevier, 2017-11-01) Aral, Hayriye; Çelik, Kadir Serdar; Altındağ, Ramazan; Aral, TarıkA novel multifunctional stationary phase based on silica gel was synthesised starting from L- isoleucine and 4-phenylbutylamine and evaluated as a hydrophilic interaction/reversed-phase mixed-mode stationary phase for high-performance liquid chromatography (HPLC). The prepared stationary phase was characterized by elemental analysis, infrared spectroscopy (IR), scanning electron microscopy (SEM), Brunauer, Emmett and Teller (BET) and solid-state 13C nuclear magnetic resonance (NMR). The mechanisms involved in the chromatographic separation are multi-interaction, including hydrophobic, π-π, hydrogen-bonding, dipole-dipole and ion-dipole interactions. Based on these interactions, successful separation could be achieved among several aromatic compounds having different polarities under both hydrophilic interaction liquid chromatography (HILIC) and reversed phase (RP) condition. Nucleotides/nucleosides were separated in the HILIC mode. The effects of different separation conditions, such as pH value, mobile-phase content, column temperature, buffer concentration and flow rate, on the separation of nucleotides/nucleosides in HILIC mode were investigated. The seven nucleotides/nucleosides were separated within 22 min, while six of them were separated within 10 min by isocratic elution. To determine the influence of the new multifunctional stationary phase under the RP condition, a number of moderately and weakly polar and nonpolar compounds, such as 10 substituted anilines and eight substituted phenols were separated successfully under the RP condition within 14 and 15 min, respectively. Additionally, nine mixtures of polar/nonpolar test compounds were simultaneously separated within 19 min, while seven of them were separated within 12 min, under HILIC/RP mixed-mode conditions. Chromatographic parameters, such as the retention factor and peak asymmetry factor, were calculated for all of the analytes, while the theoretical plate number was calculated for analytes separated by isocratic elution. Compared to traditional C18 and commercial HILIC columns, the new stationary phase exhibited both HILIC and RPLC performance, and the scope of analyte separation was thus enlarged.Öğe Synthesis of a mixed-model stationary phase derived from glutamine for HPLC separation of structurally different biologically active compounds: HILIC and reversed-phase applications(Elsevier, 2015-01) Aral, Tarık; Aral, Hayriye; Ziyadanoğulları, Berrin; Ziyadanoğulları, RecepA novel mixed-mode stationary phase was synthesised starting from N-Boc-glutamine, aniline and spherical silica gel (4 μm, 60 Å). The prepared stationary phase was characterized by IR and elemental analysis. The new stationary phase bears an embedded amide group into phenyl ring, highly polar a terminal amide group and non-polar groups (phenyl and alkyl groups). At first, this new mixed-mode stationary phase was used for HILIC separation of four nucleotides and five nucleosides. The effects of different separation conditions, such as pH value, mobile phase and temperature, on the separation process were investigated. The optimum separation for nucleotides was achieved using HILIC isocratic elution with aqueous mobile phase and acetonitrile with 20 °C column temperature. Under these conditions, the four nucleotides could be separated and detected at 265 nm within 14 min. Five nucleosides were separated under HILIC isocratic elution with aqueous mobile phase containing pH=3.25 phosphate buffer (10 mM) and acetonitrile with 20 °C column temperature and detected at 265 nm within 14 min. Chromatographic parameters as retention factor, selectivity, theoretical plate number and peak asymmetry factor were calculated for the effect of temperature and water content in mobile phase on the separation process. The new column was also tested for nucleotides and nucleosides mixture and six analytes were separated in 10 min. The chromatographic behaviours of these polar analytes on the new mixed-model stationary phase were compared with those of HILIC columns under similar conditions. Further, phytohormones and phenolic compounds were separated in order to see influence of the new stationary phase in reverse phase conditions. Eleven plant phytohormones were separated within 13 min using RP-HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10 mM) and acetonitrile with 20 °C column temperature and detected at 230 or 278 nm. The best separation conditions for seven phenolic compounds was also achieved using reversed-phase HPLC gradient elution with aqueous mobile phase containing pH=2.5 phosphate buffer (10 mM) and acetonitrile with 20 °C column temperature and seven phenolic compounds could be separated and detected at 230 nm within 16 min.Öğe Development of a novel amide silica stationary phase for the reversed phase HPLC separation of different classes of phytohormones(Journals & Books, 2013-05-14) Aral, Tarık; Aral, Hayriye; Ziyadanoğulları, Berrin; Ziyadanoğulları, RecepA novel amide-bonded silica stationary phase was prepared starting fromN-Boc-phenylalanine, cyclo-hexylamine and spherical silica gel (4mm, 60 Å). The amide ligand was synthesised with high yield. Theresulting amide bonded stationary phase was characterised by SEM, IR and elemental analysis. Theresulting selector bearing a polar amide group is used for the reversed-phase chromatography separationof different classes of thirteen phytohormones (plant hormones). The chromatographic behaviours ofthese analytes on the amide-silica stationary phase were compared with those of RP-C18 column undersame conditions. The effects of different separation conditions, such as mobile phase, pH value,flow rateand temperature, on the separation and retention behaviours of the 13 phytohormones in this systemwere studied. The optimum separation was achieved using reversed-phase HPLC gradient elution with anaqueous mobile phase containing pH¼6.85 potassium phosphate buffer (20 mM) and acetonitrile with a221C column temperature. Under these experimental conditions, the 12 phytohormones could beseparated and detected at 230 or 270 nm within 26 minÖğe Evaluation of drilling performances of nanocomposites reinforced with graphene and graphene oxide(Springer Nature, 2018-09-16) Çelik, Yahya Hışman; Kılıçkap, Erol; Koçyiğit, NihayetThe use of graphene (G) and graphene oxide (GO) reinforced nanocomposites have a great importance since G and GO improve the interface conditions of composite materials. However, the effects of G and GO on some mechanical properties and machinability in nanocomposites are still a research topic. In this study, G was converted to GO by Hummers’ method. G and GO nanoparticles were added to epoxy at different ratios and the tensile strengths of nanocomposites were determined. By taking into account, the reinforcement ratio of nanocomposites having the highest tensile strength, epoxy with G and GO, and unreinforced epoxy were added to carbon fiber (CF) fabric by hand lay-up. Thus, fabrication of the carbon fiber-reinforced plastic (CFRP) composite, and the G/CFRP and GO/CFRP nanocomposites was carried out. The effects of the G and GO on the fabricated nanocomposites, and the effect of different drilling parameters (cutting speed and feed rate) on the cutting force, cutting torque, temperature, and delamination factor were investigated. In the drilling of these composites, drills with the different bit point angles and the diameter of 5 mm were used. As a result, it was observed that GO was successfully synthesized, and G and GO positively affected the tensile strength, and GO exhibited a more effective feature than G on the tensile strength. It was also seen that the increase of the cutting speed, feed rate, bit point angle caused the increase in the cutting forces, cutting torque, and delaminations.
