Yeni bir Hidrofilik Etkileşim/Ters Faz Karışık-Mod Sıvı Kromatografik Sabit Fazın Sentezi ve Karakterizasyonu

L-izolözin ve 2-aminoasetanilitten yola çıkılarak amid-silika tabanlı çok fonksiyonlu yeni bir dolgu maddesi sentezlendi. Bu vesile ile bileşik 1, 2, 3 ve 4 ilk kez sentezlenmiş olup bileşik 1, 2 ve 4’ün ayrıntılı karakterizasyonları yapılmıştır. Dolgu maddesi güvenilir ve tekrarlanabilir bir yöntemle sentezlenmiş olup yapısı katı faz 13C NMR, taramalı elektron mikroskobisi (SEM), ve Brunauer, Emmett and Teller (BET) ile doğrulandı. Yeni geliştirilen bu dolgu maddesi polar grup olarak dört amid grubu, apolar gruplar olarak da aromatik halka ve alifatik zincir içerir. Bu nedenle, bu dolgu maddesi hem hidrofilik etkileşim (HILIC) hem de ters faz (RPLC) sıvı kromatografisinde kullanılabilir. Dolgu maddesinin L-izolözinden sentezlendiği için aynı zamanda kiraldir ve normal faz kromatografide rasemik bileşiklerin enantiyomerik ayrılmasında kullanılabilir.

Synthesis and Characterisation of a New Hydrophilic Interaction/Reversed Phase Mixed-Mode Chromatographic Stationary Phase

Anovel multifunctional stationary phase based the amide-silica was synthesised starting from L-isoleucine and 2-aminoacetanilide. Hereby, compounds 1, 2, 3 and 4 were synthesised for the first time and 1, 2 and 4 were identified. The stationary phase was synthesised by a reliable and repeatable method and characterized by elemental analysis, solid state 13C NMR, scanning electron microscope (SEM), and Brunauer, Emmett and Teller (BET). This stationary phase possess four amide groups as polar cites, phenyl ring as aromatic non-polar cite and isopropyl as an aliphatic non-polar cite. Therefore, it can act as both hydrophilic interaction (HILIC) and reversed phase (RPLC) chromatographic stationary phase. The stationary phase has also chirality and can be used in enantioseparation of racemic compounds in normal phase chromatography (NPLC).

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