J. Wegmann et al., Poly(ethylene-co-acrylic acid) stationary phases for the separation of shape constrained isomers, ANALYT CHEM, 73(8), 2001, pp. 1814-1820
A new approach for the synthesis of long alkyl chain length stationary phas
es for use in reversed-phase liquid chromatography is described. Poly(ethyl
ene-co-acrylic acid) copolymers (i.e., (-CH2CH2-)(x)[CH2CH(CO2H)-](y)) with
different levels of acrylic acid were covalently bonded to silica via glyc
idoxypropyl or aminopropyl linkages. C-13 cross polarization magic angle sp
inning (CP/MAS) nuclear magnetic resonance (NMR) spectroscopy was used to c
haracterize the new reversed-phase materials. Aspects of shape selectivity
were evaluated for six different columns with Standard Reference Material (
SRM) 869a, Column Selectivity Test Mixture for liquid Chromatography, Selec
tivity for isomer separations was enhanced for stationary phases prepared w
ith poly(ethylene-co-acrylic acid) containing a mass fraction of 5% acrylic
acid. The relationship between alkyl conformation and chromatographic prop
erties was studied by C-13 magic angle spinning (MAS) NMR measurements, and
correlations were made with the composition of the polymer. Finally, the e
ffectiveness of this phase is demonstrated by the separation of several bet
a -carotene isomers.