Imobilização por radiação gama de fase estacionaria liquida sobre suporte de silica para uso em cromatografia liquida de alta eficiencia (CLAE)

AUTOR(ES)
DATA DE PUBLICAÇÃO

1992

RESUMO

At present, High Performance Liquid Chromatography (HPLC) is among the most important analytical techniques because of its high separation ability, sensitivity, rapidity and versatility. The success of chromatographic separation as well as its range of applicability is determined by the choice of the chromatographic column and, therefore, of the stationary phase there in. This stationary phase is generally imported an of the high cost. With the intent of minimizing this factor and to investigate the process of imrnobilization, by gamma radiation, a liquid stationary phase (polimethyloctylsiloxane) was immobilized on a support (silica gel) using different gamma radiation doses. After irradiation, the packing material attained a greater thermal stability and was more resistant to solvent extraction and the chromatographic rinsing with the mobile phase. This last characteristic permits the recuperation of contaminated columns since it is possible to wash them without removing a significative quantity of the immobilized liquid stationary phase. The chromatographic performance of columns packed with irradiated packing material was superior to that obtained with packing not submitted to irradiation. Possible, this is due to the crosslinking resulting from gamma irradiation, which causes a greater shielding of the residual hydroxyl groups. The efficiency obtained with the columns packed with the prepared packing material was unaltered during some time, indicating that in addition to the efficiency of the irradiation, the packing method used was very good. Gamma radiation was shown to produce efficient immobilization of the liquid stationary phase, a dose of 120 kGy being that which resulted in better values of the chromatographics parameters. The cost of the prepared stationary phase is 90% cheaper than comercial phase, showing that an efficient and economical method of stationary phase preparation for reversed phase for HPLC was achieved.

ASSUNTO(S)

cromatografia liquida analise cromatografica

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