Cemil AYDOĞAN, Fatma YILMAZ, Duygu ÇİMEN, Müge ANDAÇ, Huma SHAİKH, Adil DENİZLİ

Sülfonamid Antibiyotiklerin Ayırımı için Hidrofilik Etkileşim Elektrokromatografi Yönteminin Kullanımı

B u çalışma hidrofilik monolitik kolonların hazırlanması ve sülfonamid antibiyotiklerin ayırımında kullanımını içermektedir. Kolon, 2-hidoksietil metakrilat HEMA , etilen dimetakrilat EDMA ve metakrilik asitin MAA toluen ve 1-dodekanol çözücü çifti eşliğinde, 100 μm iç çaplı i.d kapiler kolon içinde tek basamaklı olarak sentezlenmesiyle hazırlandı. Monolitik kolon, hem elektrokromatografik olarak hemde taramalı elektron mikroskobu SEM ile karakterize edildi. Hazırlanan kolon tiyoüre ve toluen’in işaretçi olarak kullanıldığı kromatografi sisteminde hidrofilik davranış göstermektedir. SEM görüntüleri, monolitik kolonun yaklaşık 2 μm çapında küresel partiküller içerdiğini göstermektedir. Hazırlanan hidrofilik monolitin, sülfonamidlerin elektrokromatografik ayırımında sabit faz olarak kullanımı yeni bir metod olarak geliştirilerek ayırım işlemi başarılı bir şekilde gerçekleştirildi. ACN miktarı, pH, iyonik şiddet gibi bazı parametrelerin sülfopiridin, sülfodiazin, sülfometazin, sülfisoksazol ve sülfadoksin gibi antibiyotiklerin ayırımına etkisi de incelendi. Yüksek organik solvent ACN>60% içeriğinde tipik bir hidrofilik etkileşim mekanizması gözetlendi

Anahtar Kelimeler:

kapiler elektrokromatografi, hidrofilik monolit, sülfonamid antibiyotikler, alıkonma mekanizması

Study on an Hydrophilic Interaction Electrochromatography Method for Separation of Sulfonamide Antibiotics

This study describes the preparation of a hydrophilic monolithic column and its application to sulfonamide antibiotics. The column was prepared by single step in situ polymerization of 2-hydroxyethyl methacrylate HEMA , ethylene dimethacrylate EDMA and methacrylic acid MAA in a binary porogenic solvent consisting of toluene and 1-dodecanol, inside a 100 μm-i.d. capillary. The resulting monolith was electrochromatographically characterized as well as SEM. The prepared column showed hydrophilic behaviour using thiourea and toluene as markers. The SEM images showed that the monolithic column composed of spherical particles of approximately 2 μm in diameter. Using this hydrophilic monolith as stationary phase, hydrophilic interaction electrochromatography of sulfonamide antibiotics as a new method was developed. The method was successfully used for the separation of sulfonamide antibiotics. Some parameters including acetonitrile ACN content, pH and ionic strength on the separation of the sulfonamides, namely sulfaprydine, sulfadiazine, sulfamethazine, sulfisoxazole and sulfadoxine were also investigated. A typical hydrophilic interaction separation mechanism was revealed at higher organic solvent content ACN > 60% .

Keywords:

Capillary electrochromatography, hydrophilic monolith, sulfonamide antibiotics, retention mechanism,

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