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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 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 Yeni geliştirilen çok fonksiyonlu mixed-mode kolon dolgu maddesinin HILIC-ters faz uygulamaları(Batman Üniversitesi Fen Bilimleri Enstitüsü, 2018-02-10) Altındağ, Ramazan; Aral, TarıkBu tez çalışmasında, daha önce başka bir yüksek lisans tezi kapsamında sentezlenip HPLC kolonu haline getirilen Ile-PBA-Mix sabit fazın HPLC ile hidrofilik etkileşim (HILIC)/ters faz (RPLC) sıvı kromatografi mixed-mod özelliği incelendi. Ile-PBA-Mix kolonunun yüksek polardan en düşük polariteye kadar farklı grupların ayrılmasında başarı ile kullanıldığı görüldü. Ile-PBA-Mix kullanılarak HILIC şartlarında nükleotid/nükleositler ve B vitaminleri ayrıldı. 6 tane nükleosid/nükleotid 10 dakikada, 6 tane B vitamin de 22 dakikada başarı ile ayrıldı. Ayrıca nükleotid/nükleosit ve B-vitaminlerinin ayrılmasına çeşitli deneysel şartların etkisi de incelendi. Kolonun ters fazdaki etkinliğini incelemek için orta polarlıktaki bileşik sınıfları olan anilinler ve fenoller kullanıldı. 9 tane anilin 14 dakikada, 9 tane fenol de 15 dakikada ters faz şartlarında ayrıldı. Bunlara ek olarak yüksek polariteye, orta polariteye ve düşük polariteye sahip 9 analit karışımı da denendi ve HILIC/RP mixed-mode mobil faz ile 19 dakikada ayrılması sağlandı. Ayrılması sağlanan bileşikler için çeşitli kromatografik parametreler (alıkonma faktörü, pik asimetri faktörü ve teorik tabaka sayısı) hesaplandı. Geleneksel C18 VE HILIC kolonlarla kıyasladığımızda, Ile-PBA-Mix kolonunu hem RPLC hem de HILIC performansı sergilediği ve geniş bir analit sınıfına uygulanabildiği görülmüştür.
