Sains Malaysiana 50(11)(2021): 3241-3250



Separation of Polar Compounds using Poly(Ethylene Oxide) Bonded Stationary Capillary Liquid Chromatography

(Pengasingan Sebatian Kutub menggunakan Kromatografi Cecair Kapilari Terikat Poli(Etilena Oksida))




1Department of Chemistry Education, Faculty of Education and Teacher Training, University of Riau, Pekanbaru, Indonesia


2Department of Chemistry, Faculty of Mathematics and Natural Sciences, IPB University, Bogor, Indonesia


3Department of Chemical Engineering, Faculty of Industrial Technology, Ahmad Dahlan University, Yogyakarta, Indonesia


4Department of Chemistry and Biomolecular Science, Faculty of Engineering, Gifu University, Gifu, Japan


Diserahkan: 21 April 2020/Diterima: 15 Mac 2021




Poly(ethylene oxide) (PEO) bonded stationary phase has been synthesized by a single and simple step reaction. Poly(ethylene glycol monomethyl ether p-toluene sulfonate) (tosylated-PEO, molecular weight 900, n ≈ 18) was chemically bonded to 3-aminopropyl silica (TSKgel NH2-60, 5 µm particle size, and 60 Å mean pore diameter). The prepared stationary phase was able to separate polar compounds such as phenolics and nucleobases in capillary liquid chromatography. The retention and separation of phenolics and nucleobases could be achieved under isocratic elution condition. Nucleobases such as thymine, adenine, uracil, uridine, cytidine and toluene and phenolics (phenol, pyrocatechol, pyrogallol) were baseline separated in less than 6 min using 98% acetonitrile and less than 7 minutes using 80% acetonitrile, respectively. We demonstrated that the retention of nucleobases as analyte decreased with decreasing eluent concentration. The retention of these polar compounds was believed to be based on dipole-dipole and/or hydrogen-bonding interactions.

Keywords: Capillary liquid chromatography; poly(ethylene oxide); polar compounds



Fasa pegun terikat poli(etilena oksida) (PEO) telah disintesis melalui tindak balas langkah tunggal dan sederhana. Poli(etilena glikol monometil eter p-toluena sulfonat) (tosilated-PEO, berat molekul 900, n ≈ 18) secara kimia terikat pada silika 3-aminopropil (TSKgel NH2-60, ukuran zarah 5 µm dan diameter liang 60%). Fasa pegun yang disediakan dapat memisahkan sebatian kutub seperti fenol dan nukleobes dalam kromatografi cecair kapilari. Pengekalan dan pemisahan fenol dan nukleobes dapat dicapai dalam keadaan elusi isokratik. Nukleobes seperti timin, adenin, urasil, uridin, sitidin dan toluena serta fenol (fenol, pirokatekol, pirogalol) dipisahkan awal dalam masa kurang dari 6 minit menggunakan 98% asetonitril dan kurang dari 7 minit masing-masing menggunakan 80% asetonitril. Kami menunjukkan bahawa pengekalan nukleobes sebagai analit menurun dengan penurunan kepekatan eluen. Pengekalan sebatian polar ini dipercayai berdasarkan interaksi ikatan dipol-dipol dan/atau hidrogen.

Kata kunci: Kromatografi cecair kapilari; polietilena oksida; sebatian kutub




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