Yeni geliştirilen çok fonksiyonlu mixed-mode kolon dolgu maddesinin HILIC-ters faz uygulamaları
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Dosyalar
Tarih
2018-02-10
Yazarlar
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Yayıncı
Batman Üniversitesi Fen Bilimleri Enstitüsü
Erişim Hakkı
info:eu-repo/semantics/openAccess
Attribution-ShareAlike 3.0 United States
Attribution-ShareAlike 3.0 United States
Özet
Bu 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.
In thise work, a novel multifunctional stationary phases synthesized under another graduate thesis was evaluated as a hydrophilic interaction/reversed-phase mixed-mode stationary phase for high-performance liquid chromatography (HPLC). Successful separation could be achieved by Ile-PBA-Mix column 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 minutes, while six of them were separated within 10 minutes 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 minutes, while seven of them were separated within 12 minutes, 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.
In thise work, a novel multifunctional stationary phases synthesized under another graduate thesis was evaluated as a hydrophilic interaction/reversed-phase mixed-mode stationary phase for high-performance liquid chromatography (HPLC). Successful separation could be achieved by Ile-PBA-Mix column 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 minutes, while six of them were separated within 10 minutes 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 minutes, while seven of them were separated within 12 minutes, 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.
Açıklama
Anahtar Kelimeler
Mixed-Mode Kromatografi, Polar Sabit Fazlar, Yüksek Performanslı Sıvı Kromatografisi, HILIC, Ters Faz, Mixed-Mode Chromatography, Mixed-Mode Stationary Phase, Hydrophilic Interaction Liquid Chromatography (HILIC), Reversed Phase Liquid Chromatography
Kaynak
WoS Q Değeri
Scopus Q Değeri
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Sayı
Künye
Altındağ, R. (2018). Yeni geliştirilen çok fonksiyonlu mixed-mode kolon dolgu maddesinin HILIC-ters faz uygulamaları. (Yayınlanmamış Yüksek Lisans Tezi). Batman Üniversitesi Fen Bilimleri Enstitüsü, Batman.
