RESUMEN
Poly(methyloctylsiloxane) (PMOS) was deposited on HPLC silica by a solvent evaporation procedure and this material was then extracted, using a good solvent for the PMOS, after different time periods, to remove unretained liquid polymer. Solvent extraction data reveal changes which occur at ambient temperature as a function of the time interval between particle loading and extraction. The quantity of PMOS remaining on the silica after extraction, as determined by elemental analysis for carbon, is attributed to strongly adsorbed polymer. This phenomenon is termed self-immobilization. Solid-state 29Si NMR spectra indicate the formation of a silicon species with a different chemical shift than the original PMOS. These new signals are attributed to a combination of different adsorbed and chemically bonded groups.
Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Polímeros/química , Siloxanos/químicaRESUMEN
A new C18 urea stationary phase was prepared by a single-step modification process through the reaction of ProntoSil spherical silica (3 microm, Bischoff) with the trifunctional alkoxysilane (CH3CH2O)3-Si-(CH2)3-NH-C(O)-NH-(CH2)17-CH3, prepared in our laboratory. The phase was characterized by elemental analysis and solid-state 29Si and 13C nuclear mangnetic resonance spectrometry. Chromatographic evaluations of the new phase in 150 x 3.9 mm HPLC columns involving the separation of different test mixtures, indicate good performance for both polar and basic mixtures and also show promising results for further applications.
Asunto(s)
Urea/química , Cromatografía Líquida de Alta Presión , Indicadores y Reactivos , Ligandos , Espectroscopía de Resonancia Magnética , Preparaciones Farmacéuticas/aislamiento & purificación , Dióxido de Silicio , Solventes , Espectrofotometría UltravioletaRESUMEN
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.