Desenvolvimento de fases estacionarias para cromatografia liquida de alta eficiencia em fase reversa a partir da adsorção e imobilização do poli(metiltetradecilsiloxano) sobre silica metalizada / Development of stationary phases for reservesed-phase hight-performance liquid chromatography by adsortion and immobilization of poly(metyltetradecysiloxane) onto metalized silica supports

AUTOR(ES)
DATA DE PUBLICAÇÃO

2006

RESUMO

This work presents the development of stationary phases for used in Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) by sorption and immobilization of poly(methyltetradecylsiloxane) (PMTDS) onto metalized (zirconized and titanized) silica supports. The preparation of metalized silica supports was optimized using experimental design. Two immobilization procedures, thermal treatment and gamma radiation, and the self-immobilization phenomenon were evaluated for preparation of the PMTDS stationary phases. The supports, PMTDS and the stationary phases were characterized by physiochemical and chromatographic tests. Si-Zr(PMTDS) and Si-Ti(PMTDS) stationary phases, independent of the immobilization procedure used, provide column efficiencies between 58,000 and 84,000 plates per meter and good separations with symmetrical peaks for apolar compounds. The presence of the metallic oxides on the chromatographic support resulted in stationary phases with accentuated acid character, principally for zirconized-silica-based stationary phases, providing poor chromatographic performance for basic compounds. However, the chemical stability of metalized silica-based stationary phases in alkaline mobile phases was prolonged about six times, compared with bare silica counterparts. Both Si-Zr(PMTDS) and Si-Ti(PMTDS) stationary phases present potential for separation of different pharmaceuticals and pesticides.

ASSUNTO(S)

metalized silica supports reversed stationary phases fases estacionarias reversas poly(metyltetradecysiloxane) high performance liquid chromatography supporte de silica metalizada poli(metiltetradecisiloxano) cromatografia liquida de alta eficiencia

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