Polystyrene bound stationary phase of excellent separation efficiency based on partially sub-2μm silica monolith particles

• Published in: Journal of Chromatography A 2013-08, Vol.1303, p.9-17
• Main Authors: Ali, Faiz, Cheong, Won Jo, ALOthman, Zeid A., ALMajid, Abdullah M.
• Format: Article
• Language: English
• Subjects: acetonitrile; Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography; coatings; Computational efficiency; Computing time; Exact sciences and technology; Exceptional high separation efficiency; heat; high performance liquid chromatography; Initiator attachment; Initiators; Other chromatographic methods; Partially sub-2 μm silica monolith particles; Polymerization; Polystyrene resins; polystyrenes; RAFT polymerization; Separation; sieving; silica; Silicon dioxide; Uniform and thin polystyrene film; washing
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2013.06.016

•Partially sub-2μm silica monolith particles with rather large pores were prepared.•Polystyrene bound monolith particles were prepared by RAFT polymerization.•The resultant phase showed very good efficiencies. Partially sub-2μm porous silica monolith particles have been synthesized by a renovated procedure and modified to polystyrene coated silica particles with excellent separation efficiency when used as chromatographic media. In the procedure of preparing silica monolith particles in this study, subtle control of formulation of the reaction mixture and multi-step heating followed by calcination, without any washing and sieving process, enabled formation of silica particles characterized by proper particle and pore size distribution for high separation efficiency. 3-Chloropropyl trimethoxysilane was used as the halogen terminal spacer to combine the initiator to silica particles. Uniform and thin coating of polystyrene layer on initiator attached silica particles was formed via reversible addition-fragmentation chain transfer (RAFT) polymerization. Micro-columns (1.0mm ID and 300mm length) were packed with the resultant phase and their chromatographic performance was elucidated by HPLC. A mobile phase of 60/40 (v/v) acetonitrile/water containing 0.1% TFA and a flow rate of 15μL/min were found to be the optimized conditions leading to number of theoretical plates close to 50,000 (165,000m–1). This is the very first study to get such highly efficient HPLC columns using a silica monolith particulate stationary phase.