Production of Raw and Ligand‐modified Silica Monolith Particles in an Enhanced Scale and their Application in High Performance Liquid Chromatography

Abstract

Porous silica monolith particles have been successfully prepared in an enhanced scale (80-85 g/batch) and derivatized with some ligands and packed in micro-columns. The separation efficiencies as high as 127 000 and 175 000 plates /m were achieved with 30 and 15 cm columns packed with C18 modified particles, respectively. The average particle size and particle size distribution were reduced by scale-up and subtle change of the formulation of reaction mixture. This phase also has shown some encouraging possibility for fast analysis. Another phase derivatized with mixed ligands of C8 and urea functionalities showed promising feasibility for proteomic analysis.

Styrene‐N‐phenylacrylamide co‐polymer modified silica monolith particles with an optimized mixing ratio of monomers as a new stationary phase for the separation of peptides in high performance liquid chromatography

“…The volume‐based PSD plots are compared between the bare and modified silica monolith particles in Figure . It is convenient to use the volume‐based d(0.5) value as the average particle size consistently for the particles of wide particle size distribution . The volume‐based d(0.5) was increased from 2.596 to 3.247 µm by co‐polymer modification.…”

“…Ligand‐modified silica monolith particles have higher separation efficiency (up to 195 000 plates/m) and permeability (2.4 × 10 −14 m 2 for 3.9 µm C18 modified silica monolith particles) than spherical porous silica particles . Their separation efficiency is comparable to that of core‐shell particles of similar average particle sizes while the resultant column back pressure is lower (roughly two‐thirds) than that of conventional spherical particles . Such phases reported in the previous studies were C18 modified and polystyrene modified phases.…”

“…The stationary phases based on ground silica monolith particles may be adopted to solve the column packing difficulties. Such stationary phases have been developed in our laboratory . Their unique character of multiple particle shapes causes a partially monolithic structure in the packed bed enabling fast slurry flux during packing to result in improved packing quality.…”

An optimized mixed‐mode stationary phase based on silica monolith particles for the separation of peptides and proteins in high‐performance liquid chromatography

“…The last strategy was to use ground silica monolith particles as the substrate for ligand modification. We have been studying ground silica monolith particles as new stationary phase media . Ground silica monolith particles, a special type of packing material, have higher permeability (2.4 × 10 −14 m 2 for 3.9 µm C18 modified silica monolith particles) and separation efficiency (up to 195 000 plates/m) than spherical porous silica particles .…”

“…Ground silica monolith particles, a special type of packing material, have higher permeability (2.4 × 10 −14 m 2 for 3.9 µm C18 modified silica monolith particles) and separation efficiency (up to 195 000 plates/m) than spherical porous silica particles . The resultant back pressure of C18 bound silica monolith particles is lower (roughly two thirds) than that of stationary phases based on spherical core‐shell particles while separation efficiency is comparable with that of core‐shell particles of similar average particle sizes . For example, the chromatographic performances of a series of columns packed with various Kinetex C18 core‐shell particles (5, 2.6, 1.7, 1.3 µm) were reported .…”