Stationary phases for reversed phase high performance liquid chromatography (RP-HPLC) based on functionalized inorganic oxide surfaces

Particles of porous silica or other solvent resistent inorganic oxides can be functionalized by aliphatic (e.g., C-8 or C-18) or other groups to give stationary phases for use in reversed phase HPLC. The functionalization can be done by bonding of individual groups to the surface of the support particles, by producing an organic polymeric film from pre-polymers, or by adsorbing/immobilizing pre-formed polymers on the surfaces. These three types of functionalization are reviewed.61662

High-performance Liquid Chromatographic Stationary Phases Based On Poly(methyloctylsiloxane) Immobilized On Silica. Ii. Chromatographic Evaluation.

This work describes the chromatographic characterization of stationary phases prepared by deposition of poly(methyloctylsiloxane) (PMOS) on silica followed by immobilization using one of several different processes: thermal treatments (120 or 220 degrees C for 4 h), microwave irradiation (495 W for 15 min), gamma radiation (dose of 80 kGy) or self-immobilization. This evaluation was based on the chromatographic parameters of several test solutes. The stationary phases immobilized at 220 degrees C and which underwent self-immobilization were not appropriate for chromatographic use but the other immobilized phases presented chromatographic performances similar in most respects to a commercial phase (Rainin C8) while the peak characteristics of the basic probe were significantly better with these phases.948109-1

High-performance Liquid Chromatographic Stationary Phases Based On Poly(methyloctylsiloxane) Immobilized On Silica. Iii. Stability Evaluations.

Several reversed-phase materials for high-performance liquid chromatography were obtained by deposition of poly(methyloctylsiloxane) (PMOS) on HPLC silica particles, followed by immobilization using different procedures. Each phase had characteristic physicochemical and chromatographic properties. The present work evaluates the stability of these phases with both neutral and basic mobile phases. All of the stationary phases were quite stable to neutral mobile phase, with less stability at higher pH. However, one thermally immobilized phase presented high stability even at an elevated temperature with a pH 10.0 mobile phase.98793-10

Stability Studies Of Stationary Phases From Poly(methyltetradecylsiloxane) Sorbed And Immobilized Onto Metalized And Unmodified Silicas.

Stationary phases for RP-HPLC were prepared from metalized (titanized and zirconized) and unmodified silica particles using sorbed and immobilized poly(methyltetradecylsiloxane) (PMTDS). Different immobilization procedures, such as gamma irradiation and thermal treatments, were used for the preparation of the immobilized PMTDS phases. The stabilities of these stationary phases were evaluated by passing alkaline (pH 10) mobile phase through 60 mm x 3.9 mm columns of the different phases, with periodic tests to evaluate chromatographic performance. The results show that higher stabilities were obtained with stationary phases based on PMTDS immobilized on zirconized silica, these phases being 50% more stable than their titanized silica counterparts and 400% more stable than those based on unmodified silica. These supports provide higher chemical stability to the laboratory-made stationary phases, when compared with chemically bonded silica-based phases.301844-5

High-performance Liquid Chromatographic Stationary Phases Based On Poly(methyloctylsiloxane) Immobilized On Silica. I. Physical And Chemical Characterizations.

Five different reversed-phase materials for high-performance liquid chromatography were obtained by deposition of poly(methyloctylsiloxane) in HPLC silica particles, followed by immobilization using different processes: thermal treatment (120 or 220 degrees C for 4 h), irradiation with microwaves (495 W for 15 min), gamma radiation (dose of 80 kGy) and self-immobilization. These phases were characterized by gel permeation chromatography, percent carbon, 13C and 29Si solid-state nuclear magnetic resonance spectroscopy, infrared spectroscopy, thermogravimetric analysis and scanning electron microscopy. The results show that the different immobilization processes produce different physical characteristics in the prepared phases.94897-10