Journal
TALANTA
Volume 198, Issue -, Pages 432-439Publisher
ELSEVIER SCIENCE BV
DOI: 10.1016/j.talanta.2019.02.046
Keywords
Chiral stationary phase; Hybrid monolith; Thiol-ene click reaction; Capillary liquid chromatography; Polyhedral oligomeric silsesquioxanes
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Funding
- China State Key Basic Research Program Grant [2016YFA0501402]
- National Science Fund for Distinguished Young Scholars [21525524]
- National Natural Science Foundation of China [21575141]
- CAS-Weigao Research & Development Program [[2017]-009]
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Although various click polymerization reactions (thiol-ene, thiol-yne, thiol-Michael, thiol-epoxy and amine epoxy) have been utilized to prepare either hybrid or organic monolithic columns with homogeneous network structures, there were few reports on fabrication of monolithic CSPs via click polymerization. Herein, a fast and robust approach was explored to fabricate cinchona-based monolithic hybrid CSPs via photo-initiated thiol-ene polymerization within 10 min in one step. A self-synthesized octakis(3-mercaptopropyl) octasilsesquioxane (POSS-SH) was polymerized with phenylisocyanate cinchonidine (PCD) and (+)-N,N'-diallyl-L-tartardiamide (DATDA) or 1,2,4-trivinylcyclohexane (TVCH). The resulting two kinds of as-synthesized monolithic CSPs, poly (POSS-co-DATDA-co-PCD) and poly(POSS-co-TVCH-co-PCD), were evaluated for cLC enantioseparation of acidic racemates. It was found that they exhibited different enantioseparation ability due to using different multivinyl crosslinkers. The influence of ACN content in mobile phase on the enantioseparation of acidic racemates was investigated. The separation mechanism was also discussed on the basis of a comparison of enantioseparation on two kinds of hybrid monolithic CSPs.
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