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Facile modification of sulfhydryl-containing hybrid core-shell silica microspheres via thiol-ene click chemistry for separation of achiral and chiral compounds.

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Τίτλος: Facile modification of sulfhydryl-containing hybrid core-shell silica microspheres via thiol-ene click chemistry for separation of achiral and chiral compounds.
Συγγραφείς: Guo T; Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi'an 710127, China., Liang J; Yulin Innovation Institute of Clean Energy, Yulin 719099, China., Xiao T; Yulin Innovation Institute of Clean Energy, Yulin 719099, China., Yan M; Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi'an 710127, China., Jiang L; Yulin Innovation Institute of Clean Energy, Yulin 719099, China., Ma S; Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences (CAS), Dalian 116023, China. Electronic address: shujuanm@163.com., Wei Y; Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi'an 710127, China., Ou J; Key Laboratory of Synthetic and Natural Function Molecule Chemistry of Ministry of Education, College of Chemistry and Materials Science, Northwest University, Xi'an 710127, China. Electronic address: junjieou@nwu.edu.cn.
Πηγή: Journal of chromatography. A [J Chromatogr A] 2026 May 24; Vol. 1775, pp. 466906. Date of Electronic Publication: 2026 Mar 17.
Τύπος έκδοσης: Journal Article
Γλώσσα: English
Στοιχεία περιοδικού: Publisher: Elsevier Country of Publication: Netherlands NLM ID: 9318488 Publication Model: Print-Electronic Cited Medium: Internet ISSN: 1873-3778 (Electronic) Linking ISSN: 00219673 NLM ISO Abbreviation: J Chromatogr A Subsets: MEDLINE
Imprint Name(s): Original Publication: Amsterdam ; New York : Elsevier, 1993-
Ιατρικοί όροι (MeSH): Silicon Dioxide*/chemistry , Click Chemistry*/methods , Sulfhydryl Compounds*/chemistry , Microspheres*, Stereoisomerism ; Liquid Chromatography-Mass Spectrometry
Περίληψη: To address the tedious preparation steps of existing thiol-functionalized chromatographic stationary phases and the scarcity of research on thiol-hybridized core-shell materials, this paper proposes a "one-pot" synthetic route for thiol-hybridized core-shell silica microspheres (SiO2@SiO2-thiol). The results demonstrated that the "one-pot" method could efficiently prepare SiO2@SiO2-thiol with excellent monodispersity, uniform thiol-hybridized shell layers and tunable pore structures. Subsequently, two types of stationary phases were constructed by utilizing a dual-pathway modification strategy, with these hybrid microspheres as the matrix. The separation performance and mechanism of these stationary phases for both achiral and chiral compounds (such as amino acid racemates) were systematically investigated. The stationary phase modified with hydrophobic 1-tetradecene (C14-thiol-UV) exhibited excellent separation performance, achieving a column efficiency of 55,180 plates m⁻¹ when using butylbenzene as a probe. Furthermore, the combination of C14-thiol-UV column with liquid chromatography-mass spectrometry (LC-MS) enabled effective analysis of perfluorinated compounds (PFASs), further verifying the applicability and practicality of the constructed stationary phase in the separation of complex samples. Meanwhile, compared with two kinds of chiral stationary phases (CSP) in our previous work, the as-prepared thiol‑t‑BuCQN column modified with tert‑butylcarbamoylquinine (t-BuCQN) in this study exhibited significantly enhanced chiral recognition capability, and baseline separation (Rs≥1.5) of 10 racemates of amino acid derivatives was achieved.
(Copyright © 2026 Elsevier B.V. All rights reserved.)
Competing Interests: Declaration of competing interest The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.
Contributed Indexing: Keywords: Achiral/chiral separation; Click chemistry; Hybrid core-shell microspheres; One-pot method
Substance Nomenclature: 7631-86-9 (Silicon Dioxide)
0 (Sulfhydryl Compounds)
Entry Date(s): Date Created: 20260321 Date Completed: 20260711 Latest Revision: 20260711
Update Code: 20260711
DOI: 10.1016/j.chroma.2026.466906
PMID: 41864060
Βάση Δεδομένων: MEDLINE
Περιγραφή
ISSN:1873-3778
DOI:10.1016/j.chroma.2026.466906