In situ polymerization of monolith based on poly(Triallyl Isocyanurate-co-trimethylolpropane triacrylate) and its application in high-performance liquid chromatography.

A novel organic monolithic stationary phase was prepared for high-performance liquid chromatography (HPLC) by in situ copolymerization. In which, triallyl isocyanurate (TAIC) and trimethylolpropane triacrylate (TMPTA) in a binary porogenic solvent consisting of polyethylene glycol 200 and 1, 2-propanediol were used. The resultant monoliths with different column properties (e.g., morphology and pressure) were optimized by adjusting the ratio of TMPTA/TAIC and the composition of porogenic solvent. The resulting poly(TAIC-co-TMPTA) monolith showed a relatively homogeneous structure, good permeability and mechanical stability. The chemical group of the monolith was assayed by the infrared spectra method, the morphology of monolithic material was studied by scanning electron microscopy and the pore size distribution was determined by a mercury porosimeter. A series of small molecules were used to evaluate the column performance in terms of hydrophobic mode. At an optimized flow rate of 1.0 mL min(-1), the theoretical plate number of analyte was >15,000 plates m(-1). These applications demonstrated that the monoliths could be successfully used as the stationary phase in conjunction with HPLC to separate small molecules from the mixture.

Preparation and characterization of poly(triallyl isocyanurate-co-trimethylolpropane triacrylate) monolith and its applications in the separation of small molecules by liquid chromatography.

A new polymeric monolith was prepared in stainless-steel column and fused-silica capillary, respectively, by atom transfer radical polymerization technique. In the polymerization, triallyl isocyanurate (TAIC) was used as the functional monomer; trimethylolpropane triacrylate (TMPTA) as the crosslinking agent; polyethylene glycol 200 and 1,2-propanediol as the co-porogens; carbon tetrachloride as the initiator and ferrous chloride as the catalyst. The conditions of polymerization were optimized. Morphology of the prepared poly(TAIC-co-TMPTA) monolith was investigated by scanning electron microscopy; pore properties were assayed by mercury porosimetry and nitrogen adsorption. The characterization indicated that the prepared reversed-phase monolith possessed uniform structure, good permeability and mechanical stability. The column was used as the stationary phase of reversed phase high performance liquid chromatography (RP-HPLC) and capillary liquid chromatography (CLC) to separate the mixture of aromatic compounds. The new column performed around 125,000 theoretical plates per meter. The column showed good reproducibility: the relative standard deviation values of the retention factor values for aromatic compounds were less than 1.52% (n=7, column-to-column).