TY  - JOUR
U1  - Zeitschriftenartikel, wissenschaftlich - begutachtet (reviewed)
A1  - Fait, Fabio
A1  - Steinbach, Julia
A1  - Kandelbauer, Andreas
A1  - Mayer, Hermann
T1  - Incorporation of silica nanoparticles into porous templates to fabricate mesoporous silica microspheres for high performance liquid chromatography applications
JF  - Journal of chromatography : including electrophoresis, mass spectrometry and other separation and detection methods. A
N2  - High-performance liquid chromatography is one of the most important analytical tools for the identification and separation of substances. The efficiency of this method is largely determined by the stationary phase of the columns. Although monodisperse mesoporous silica microspheres (MPSM) represent a commonly used material as stationary phase their tailored preparation remains challenging. Here we report on the synthesis of four MPSMs via the hard template method. Silica nanoparticles (SNPs) which form the silica network of the final MPSMs were generated in situ from tetraethyl orthosilicate (TEOS) in the presence of (3-aminopropyl) triethoxysilane (APTES) functionalized p(GMA-co-EDMA) as hard template. Methanol, ethanol, 2-propanol, and 1-butanol were applied as solvents to control the size of the SNPs in the hybrid beads (HB). After calcination, MPSMs with different sizes, morphology and pore properties were obtained and characterized by scanning electron microscopy, nitrogen adsorption and desorption measurements, thermogravimetric analysis, solid state NMR and DRIFT IR spectroscopy. Interestingly, the 29Si NMR spectra of the HBs show T and Q group species which suggests that there is no covalent linkage between the SNPs and the template. The MPSMs were functionalized with trimethoxy (octadecyl) silane and used as stationary phases in reversed-phase chromatography to separate a mixture of eleven different amino acids. The separation characteristics of the MPSMs strongly depend on their morphology and pore properties which are controlled by the solvent during the preparation of the MPSMs. Overall, the separation behavior of the best phases is comparable with those of commercially available columns. The phases even achieve faster separation of the amino acids without loss of quality.
KW  - polymer template method
KW  - high performance liquid chromatography (HPLC)
KW  - siloxane functionalized polymer
KW  - mesoporous silica microspheres
Y1  - 2023
SN  - 0021-9673
SS  - 0021-9673
U6  - https://doi.org/10.1016/j.chroma.2023.464190
DO  - https://doi.org/10.1016/j.chroma.2023.464190
VL  - 1705
SP  - 1
EP  - 8
S1  - 8
PB  - Elsevier
CY  - Amsterdam
ER  -