raffinose and acrylic-acid

Monolithic silica capillary columns for hydrophilic interaction liquid chromatography (HILIC) were prepared by on-column polymerization of acrylic acid on monolithic silica in a fused silica capillary modified with anchor groups. The products maintained the high permeability (K=5 x 10(-14)m(2)) and provided a plate height (H) of less than 10 microm at optimum linear velocity (u) and H below 20 microm at u=6mm/s for polar solutes including nucleosides and carbohydrates. The HILIC mode monolithic silica capillary column was able to produce 10000 theoretical plates (N) with column dead time (t(0)) of 20s at a pressure drop of 20 MPa or lower. The total performance was much higher than conventional particle-packed HILIC columns currently available. The gradient separations of peptides by a capillary LC-electrospray mass spectrometry system resulted in very different retention selectivity between reversed-phase mode separations and the HILIC mode separations with a peak capacity of ca. 100 in a 10 min gradient time in either mode. The high performance observed with the monolithic silica capillary column modified with poly(acrylic acid) suggests that the HILIC mode can be an alternative to the reversed-phase mode for a wide range of compounds, especially for those of high polarity in isocratic as well as gradient elution.

Topics: Acrylates; Chromatography, Liquid; Nucleosides; Polymers; Raffinose; Reproducibility of Results; Silicon Dioxide; Spectrometry, Mass, Electrospray Ionization; Sucrose; Trehalose

A novel biocompatible polyelectrolyte poly(vinyl raffinose-co-acrylic acid) (PRCA) containing a raffinose branch was prepared via redox polymerization using Fe(2+)/K(2)S(2)O(8)/H(2)O(2) starting from enzymatically-synthesized monomer: 1-O-vinyldecanedioyl raffinose. Copolymers with different monomer feed ratios were prepared and characterized with IR, NMR, and GPC. PRCA can be alternated with polycation to form microcapsules on a crystals template by electrostatic layer-by-layer technique. The multilayers of PRCA/poly(methacryloyloxyethyl dimethylbenzyl ammonium chloride) (PMBA) on quartz slides and PRCA/poly(dimethyldiallyl ammonium chloride) (PDDA) on acyclovir crystals template were fabricated and characterized with UV-Vis spectra, the microelectrophoretic measurement, and TEM. Hollow capsules can be formed after the removal of acyclovir crystals template in a buffer solution. The nano-capsule-carrying galactose residue is a potential targeting drug-controlled delivery systems.

Topics: Acrylates; Acyclovir; Biocompatible Materials; Chromatography, Gel; Drug Delivery Systems; Magnetic Resonance Spectroscopy; Microscopy, Electron, Transmission; Microspheres; Polyethylenes; Quaternary Ammonium Compounds; Raffinose; Spectrophotometry, Ultraviolet; Spectroscopy, Fourier Transform Infrared