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Preparation of Hybrid Monolithic Columns via "One-Pot" Photoinitiated Thiol-Acrylate Polymerization for Retention-Independent Performance in Capillary Liquid Chromatography
Zhang, Haiyang1,2; Ou, Junjie1; Liu, Zhongshan1,3; Wang, Hongwei1,3; Wei, Yinmao2; Zou, Hanfa1
Source PublicationANALYTICAL CHEMISTRY
2015-09-01
DOI10.1021/acs.analchem.5b01707
Volume87Issue:17Pages:8789-8797
Indexed BySCI
SubtypeArticle
WOS HeadingsScience & Technology ; Physical Sciences
WOS SubjectChemistry, Analytical
WOS Research AreaChemistry
WOS KeywordPOLYHEDRAL OLIGOMERIC SILSESQUIOXANE ; RING-OPENING POLYMERIZATION ; ENE CLICK CHEMISTRY ; SMALL MOLECULES ; STATIONARY PHASES ; REVERSED-PHASE ; SEPARATION ; ELECTROCHROMATOGRAPHY ; FUNCTIONALIZATION ; MORPHOLOGY
AbstractA novel "one-pot" approach was developed for ultrarapid preparation of various hybrid monolithic columns in UV-transparent fused-silica capillaries via photoinitiated thiol acrylate polymerization of an acrylopropyl polyhedral oligomertic silsesquioxane (acryl-POSS) and a monothiol monomer (1-octadecanethiol or sodium 3-mercapto-l-propanesulfonate) within 5 min, in which the acrylate not only homopolymerizes, but also couples with the thiol. This unique combination of two types of free-radical reaction mechanisms offers a simple way to fabricate various acrylate-based hybrid monoliths. The physical characterization, including scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy, and thermal gravimetric analysis was performed. The results indicated that the monothiol monomers were successfully incorporated into acryl-POSS-based hybrid monoliths. The column efficiencies for alkylbenzenes on the C18-functionalized hybrid monolithic column reached to 60;000-73 500 plates/m at the velocity of 0.33 mm/s in capillary liquid chromatography, which was far higher than that of previously reported POSS-based columns prepared via thermal-initiated free-radical polymerization without adding any thiol monomers. By plotting the plate height (H) of the alkylbenzenes versus the linear velocity (u) of the mobile phase, the results revealed a retention-independent efficient performance of small molecules in the isocratic elution. These results indicated that more homogeneous hybrid monoliths formed via photoinitiated thiol acrylate polymerization; particularly, the use of the multifunctional cross-linker possibly prevented the generation of gel-like micropores, reducing mass transfer resistance (C-term). Another sulfonate-containing hybrid monolithic column also exhibited hydrophobicity and ion-exchange mechanism, and the dynamic binding capacity was calculated as 71.1 ng/cm (75 mu m i.d.).
Language英语
WOS IDWOS:000360773100029
Citation statistics
Document Type期刊论文
Identifierhttp://cas-ir.dicp.ac.cn/handle/321008/146528
Collection中国科学院大连化学物理研究所
Affiliation1.Chinese Acad Sci, Dalian Inst Chem Phys, Key Lab Separat Sci Analyt Chem, Dalian 116023, Peoples R China
2.NW Univ Xian, Coll Chem & Mat Sci, Minist Educ, Key Lab Synthet & Nat Funct Mol Chem, Xian 710069, Peoples R China
3.Univ Chinese Acad Sci, Beijing 100049, Peoples R China
Recommended Citation
GB/T 7714
Zhang, Haiyang,Ou, Junjie,Liu, Zhongshan,et al. Preparation of Hybrid Monolithic Columns via "One-Pot" Photoinitiated Thiol-Acrylate Polymerization for Retention-Independent Performance in Capillary Liquid Chromatography[J]. ANALYTICAL CHEMISTRY,2015,87(17):8789-8797.
APA Zhang, Haiyang,Ou, Junjie,Liu, Zhongshan,Wang, Hongwei,Wei, Yinmao,&Zou, Hanfa.(2015).Preparation of Hybrid Monolithic Columns via "One-Pot" Photoinitiated Thiol-Acrylate Polymerization for Retention-Independent Performance in Capillary Liquid Chromatography.ANALYTICAL CHEMISTRY,87(17),8789-8797.
MLA Zhang, Haiyang,et al."Preparation of Hybrid Monolithic Columns via "One-Pot" Photoinitiated Thiol-Acrylate Polymerization for Retention-Independent Performance in Capillary Liquid Chromatography".ANALYTICAL CHEMISTRY 87.17(2015):8789-8797.
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