PMID- 37419014
OWN - NLM
STAT- MEDLINE
DCOM- 20230809
LR  - 20230809
IS  - 1873-3778 (Electronic)
IS  - 0021-9673 (Linking)
VI  - 1705
DP  - 2023 Aug 30
TI  - Incorporation of silica nanoparticles into porous templates to fabricate 
      mesoporous silica microspheres for high performance liquid chromatography 
      applications.
PG  - 464190
LID - S0021-9673(23)00416-8 [pii]
LID - 10.1016/j.chroma.2023.464190 [doi]
AB  - 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 (29)Si 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.
CI  - Copyright (c) 2023. Published by Elsevier B.V.
FAU - Fait, Fabio
AU  - Fait F
AD  - Institute of Inorganic Chemistry, University of Tubingen, Auf der Morgenstelle 
      18, Tubingen 72076, Germany; Process Analysis and Technology (PA&T), Reutlingen 
      Research Institute, Reutlingen University, Alteburgstrasse 150, Reutlingen 72762, 
      Germany.
FAU - Steinbach, Julia C
AU  - Steinbach JC
AD  - Institute of Inorganic Chemistry, University of Tubingen, Auf der Morgenstelle 
      18, Tubingen 72076, Germany; Process Analysis and Technology (PA&T), Reutlingen 
      Research Institute, Reutlingen University, Alteburgstrasse 150, Reutlingen 72762, 
      Germany.
FAU - Kandelbauer, Andreas
AU  - Kandelbauer A
AD  - Process Analysis and Technology (PA&T), Reutlingen Research Institute, Reutlingen 
      University, Alteburgstrasse 150, Reutlingen 72762, Germany; Institute of Wood 
      Technology and Renewable Materials, Department of Material Sciences and Process 
      Engineering (MAP), University of Natural Resources and Life Sciences, 
      Gregor-Mendel-Strasse 33, Vienna 1180, Austria.
FAU - Mayer, Hermann A
AU  - Mayer HA
AD  - Institute of Inorganic Chemistry, University of Tubingen, Auf der Morgenstelle 
      18, Tubingen 72076, Germany. Electronic address: hermann.mayer@uni-tuebingen.de.
LA  - eng
PT  - Journal Article
DEP - 20230701
PL  - Netherlands
TA  - J Chromatogr A
JT  - Journal of chromatography. A
JID - 9318488
RN  - 7631-86-9 (Silicon Dioxide)
RN  - 0 (Solvents)
RN  - 31743-77-8 (GMA-EDMA)
RN  - 0 (Amino Acids)
SB  - IM
MH  - Chromatography, High Pressure Liquid/methods
MH  - *Silicon Dioxide/chemistry
MH  - Microspheres
MH  - Porosity
MH  - Solvents/chemistry
MH  - *Nanoparticles/chemistry
MH  - Amino Acids
OTO - NOTNLM
OT  - (29)Si solid state NMR
OT  - High performance liquid chromatography (HPLC)
OT  - Mesoporous silica microspheres
OT  - Polymer template method
OT  - Siloxane functionalized polymer
COIS- Declaration of Competing Interest The authors declare the following financial 
      interests/personal relationships which may be considered as potential competing 
      interests: Hermann A. Mayer reports equipment, drugs, or supplies was provided by 
      Dr. Maisch GmbH.
EDAT- 2023/07/08 10:42
MHDA- 2023/08/09 06:43
CRDT- 2023/07/07 18:08
PHST- 2023/02/20 00:00 [received]
PHST- 2023/06/28 00:00 [revised]
PHST- 2023/06/30 00:00 [accepted]
PHST- 2023/08/09 06:43 [medline]
PHST- 2023/07/08 10:42 [pubmed]
PHST- 2023/07/07 18:08 [entrez]
AID - S0021-9673(23)00416-8 [pii]
AID - 10.1016/j.chroma.2023.464190 [doi]
PST - ppublish
SO  - J Chromatogr A. 2023 Aug 30;1705:464190. doi: 10.1016/j.chroma.2023.464190. Epub 
      2023 Jul 1.