A new thermally immobilized fluorinated stationary phase for RP‐HPLC

Abstract

A new fluorinated stationary phase was prepared through thermal immobilization of poly(methyl-3,3,3-trifluoropropylsiloxane) onto 5 microm Kromasil silica particles. The best conditions of immobilization time and temperature were determined through a central composite design and response surface methodologies. Physical-chemical characterization using solid-state (29)Si NMR measurements, infrared spectroscopy and elemental analysis showed that the immobilization process was effective to promote a coating of the support that corresponds to a monolayer of polymer. The stationary phase presents selectivity for positional isomers and good peak shape for basic compounds.

Synthesis, characterisation and chromatographic evaluation of pentafluorophenyl and phenyl bonded silica phases prepared using supercritical carbon dioxide as a reaction solvent

“…Curosil PFP (˛C H 2 = 1.27), Fluophase PFP (˛C H 2 = 1.23), ACE Phenyl (˛C H 2 = 1.26), XTerra Phenyl (˛C H 2 = 1.28) and to alkyl fluorinated phases, e.g. octyl fluorinated (˛C H 2 = 1.24), a fluorinated phase prepared by thermal immobilisation of poly (methyl-3,3,3-trifluoropropylsiloxane onto 5 m Kromasil silica (˛C H 2 = 1.5) and Kromasil C 18 (˛C H 2 = 1.48) [76].…”

Some new selective stationary phases for RP‐HPLC

“…In view of this, the development of a limited number of stationary phases that possess the characteristics necessary to enable separation of a vast gamut of different compounds presenting diverse properties, once an important goal, has been replaced by the task of preparing more specialized stationary phases. Among these, stationary phases with polar embedded groups 6, 32, 44, 45, aromatic ligands 46–52 and fluorinated groups 42, 53–61 can be mentioned, as well as the newer mixed mode 49, 62–65 and hydrophilic interaction phases 66–68. Immobilized polymer stationary phases having phenyl and fluorinated groups have been prepared and evaluated by LabCrom.…”

Fases estacionárias modernas para cromatografia líquida de alta eficiência em fase reversa

“…O resultado deste estudo mostrou que a FE fluorada apresentou maior interação com os compostos fluorados que as FE não fluoradas. Estes resultados despertaram o interesse em investigar estas FE e uma série de estudos [95][96][97][98][99][100][101] estão sendo realizados em vista da especificidade destas FE, principalmente comparando-as com as FE não fluoradas.…”

“…[98][99][100][101] Um exemplo deste tipo está ilustrado na Figura 6, na qual estão apresentados os cromatogramas da separação de uma mistura de difluorfenóis, que são isômeros de posição, em uma coluna recheada com uma FE fluorada e em uma coluna recheada com uma FE C8 empregando as mesmas condições cromatográficas. Os cromatogramas resultantes mostram que apenas a FE fluorada foi seletiva para a separação de todos os compostos, e, além disso, em um menor tempo de análise.…”