Monodispers-Gözenekli Polimer Mikropartiküller Üzerinde Tiyol-En Kimyası Kullanılarak Glutatyon ile Fonksiyonelleştirilmiş HILIC Sabit Fazı

Tiyol-en kimyası kullanılarak glutatyon ile fonksiyonelleştirilmiş eşboyutlu-gözenekli mikropartiküller, hidrofilik etkileşim kromatografisi için yeni bir sabit faz olarak sentezlenmiştir. Monodispers-gözenekli poli (3-trimetoksisililpropilmetakrilatco-etilendimetakrilat), poli(TMSPM-co-EDMA) mikropartiküller (boyut olarak 6 mikron), farklı çıkış lateksi/monomer ve diluent bileşimleri ile çok basamaklı mikrosüspansiyon kopolimerizasyonu ile elde edilmiştir. Tiyol ucu içeren zwitterionik kromatografik ligand (glutatyon), TMSPM bağlı poli (TMSPM-co-EDMA) mikropartiküller üzerine kovalent olarak bağlanmıştır. Seçilen başlangıç materyali, zwitteriyonik kromatografik ligandın, tiyolen kimyası kullanılarak destek materyali üzerine doğrudan bağlanmasına olanak sağlamıştır. Türevlendirilmiş mikropartiküller, 2 mm iç çapa sahip mikrobor kolonlar içerisine dolgulanmış ve hidrofilik etkileşim kromatografisinde 54000 plaka/m plaka sayısı ile nükleositlerin ayrılması için sabit faz olarak kullanılmıştır. Sonuçlar, yüksek verimlilikle hidrofilik sıvı kromatografisi uygulamaları için kromatografik sabit fazın üretiminde poli(TMSPM-co-EDMA) mikropartiküllerin ve tiyol-en kimyasının kullanılabileceğini göstermiştir.

A HILIC Stationary Phase Functionalized with Glutathione by Thiol-Ene Chemistry on Monodisperse-Porous Polymer Microparticles

Monodisperse-porous microparticles functionalized with glutathione by thiol-ene chemistry were synthesized as a newstationary phase for hydrophilic interaction chromatography. Monodisperse-porous poly(3-trimethoxysilylpropylmethacrylate-co-ethylene dimethacrylate), poly(TMSPM-co-EDMA) microspheres (6 μm in size) were obtained with different seed latex/monomer ratios and diluent compositions by multistage microsuspension copolymerization. The zwitterionic chromatographic ligand containing thiol moiety (i.e. glutathione) were covalently attached onto the TMSPM attachedpoly(TMSPM-co-EDMA) microparticles. The selected starting material allowed the direct attachment of zwitterionic ligandonto the support material using thiol-ene chemistry. The derivatized microparticles were slurry packed into the microborecolumns with 2 mm i.d. and used as stationary phase for the separation of nucleosides in hydrophilic interaction chromatography with the plate numbers up to 54.000 plates/m. The results showed the usability of tailored poly (TMSPM-co-EDMA)microparticles as a stationary phase and thiol-ene chemistry in the manufacture of a chromatographic stationary phasewith high efficiency in hydrophilic liquid chromatography applications.

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