Polycyrene-based Microbore Monolith Column Preparation for Separation of Alkylbenzene Using High Performance Liquid Chromatography

Aprilia Nur Tasfiyati, Wigang Solandjari, Elvina Dhiatul Iftitah, Akhmad Sabarudin

Abstract


In this study, polystyrene-based monolith was developed as reversed phase column in high performance liquid chromatography (HPLC) for separation of small molecule sample (alkylbenzene). Polystyrene-based monolithic column was prepared in microbore silicosteel column (100 x 1.02 mm i.d.) by in-situ polymerization reaction using styrene as monomer, divinylbenzene as crosslinker, porogenic solvents, with the presence of radical initiator 2,2’-azobis(isobutyronitrile). The morphology of the monolithic column was studied by SEM. The properties of the monolithic column, such as permeability, mechanical stability, binding capacity and pore size distribution, were characterized in detail. From the characterization results of 9 monolith variation, monolith PS-DVB with %T 30, %C 50, using toluene:1-decanol (3:7 v/v) as porogenic solvent was found to be the ideal composition and gave the best separation of alkylbenzene. It has theoretical plate value (N) of 17260/m column, also has relatively equal proportion of flow-through pore and mesopores (47% and 44% respectively). The performance of monolithic column was also compared with commercially available monolithic column Proswift RP-4H. PS-DVB monolith prepared in this study shown its superiority over commercial one.


Keywords


monolithic column; microbore; polystyrene; reversed phase liquid chromatography; alkylbenzene

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References


Urban, J., S. Eeltink, P. Jandera, P.J. Schoenmakers (2008), Characterization of polymer-based monolithic capillary columns by inverse size-exclusion chromatography and mercury-intrusion porosimetry, J. Chromatogr. A, 1182, 161-168.

Sabarudin, A., J. Huang, S. Shu, S. Sakagawa, T. Umemura (2012). Preparation of methacrylate-based anion-exchange monolithic microbore column for chromatographic separation of DNA fragments and oligonucleotides, Anal. Chim. Acta, 736, 108-114.

Ueki, Y., T. Umemura, J. Li, T. Odake, K.I. Tsunoda (2004), Preparation and application of methacrylate-based cation-exchange monolithic columns for capillary ion chromatography, Anal. Chem., 76, 7007-7012.

Nema, T., E.C.Y. Chan, P.C. Ho (2014), Applications of monolithic materials for sample preparation, J. Pharmaceut. Biomed., 87, 130-141.

Schaller, D., E.F. Hilder, P.R. Haddad (2006), Monolithic stationary phases for fast ion chromatography and capillary electrochromatography of inorganic ions, J. Sep. Sci., 29, 1705-1719.

Arrua, R.D., M. Talebi, T.J. Causon, E.F. Hilder (2012), Review of recent advances in the preparation of organic polymer monoliths for liquid chromatography of large molecules, Anal. Chim. Acta, 738, 1-12.

Urban, J., F. Svec, J.M.J. Fréchet (2010), Efficient separation of small molecules using a large surface area hyper-crosslinked monolithic polymer capillary column, Anal. Chem., 82, 1621-1623.

Zhang, Y.P., W. Li, X.J. Wang, L.B. Qu, G.L. Zhao, Y.X. Zhang (2009), Fast preparation of polystyrene-based monolith using microwave irradiation for micro-column separation, Anal. Bioanal. Chem., 394, 617–623.

Levkin, P.A., S. Eeltink, T.R. Stratton, R. Brennen, K. Robotti, H. Yin, K. Killeen, F. Svec, J.M.J. Fréchet (2008), Monolithic porous polymer stationary phases in polyimide chips for the fast high performance liquid chromatography separation of proteins and peptides, J. Chromatogr. A, 1200, 55-61.

Krenkova, J., A. Gargano, N.A. Lacher, J.M. Schneiderheinze, F. Svec (2009), High binding capacity surface grafted monolithic columns for cation exchange chromatography of proteins and peptides, J. Chromatogr. A, 1216, 6824-6830.

Huang, H.Y., Y.C. Liu, Y.J. Cheng (2008), Development of capillary electrochromatography with poly-(styrene-divinylbenzene-vinyl benzene sulfonic acid) monolith as the stationary phase, J. Chromatogr. A, 1190, 263-270.

Huang H.Y., I.Y. Huang, H.Y. Lin (2006), Separation of parabens in capillary electrochromatography using poly-(styrene-divinyl benzene-methacrylic acid) monolithic columns, J. Sep. Sci., 29, 2038–2048.

Huang H.Y., H.Y. Lin, S.P. Lin (2006), CEC with monolithic poly(styrene-divinylbenzene-vinylsulfonic acid) as the stationary phase, Electrophoresis, 27, 4674–4681.

Shu, S., H. Kobayashi, N. Kojima, A. Sabarudin, T. Umemura (2011), Preparation and characterization of lauryl methacrylate-based monolithic microbore column for reversed-phase liquid chromatography, J. Chromatogr. A, 1218, 5228-5234.

Shu, S., H. Kobayashi, M. Okubo, A. Sabarudin, M. Butsugan, T. Umemura (2012), Chemical anchoring of lauryl methacrylate-based reversed phase

monolith to 1/16” o.d. polyetheretherketone tubing, J. Chromatogr. A, 1242, 59-66.

Umemura, T., Y. Ueki, K. Tsunoda, A. Katakai, M. Tamada, H. Haraguchi (2006), Preparation and characterization of methacrylate-based semi-micro monoliths for high-throughput bioanalysis, Anal. Bioanal. Chem., 386 566-571.

Al-Bokari, M., D. Cherrak, G. Guiochon (2002), Determination of the porosities of monolithic columns by inverse size-exclusion chromatography, J. Chromatogr. A, 975, 275-284.

Bystrom, E. (2009), Porous polymeric materials for chromatography : Synthesis, functionalization and characterization, Department of Chemistry, Umea University.




DOI: http://dx.doi.org/10.21776/ub.natural-b.2015.003.02.1

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