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题名: Preparation of Hybrid Monolithic Columns via "One-Pot" Photoinitiated Thiol-Acrylate Polymerization for Retention-Independent Performance in Capillary Liquid Chromatography
作者: Zhang, Haiyang1, 2;  Ou, Junjie1;  Liu, Zhongshan1, 3;  Wang, Hongwei1, 3;  Wei, Yinmao2;  Zou, Hanfa1
刊名: ANALYTICAL CHEMISTRY
发表日期: 2015-09-01
DOI: 10.1021/acs.analchem.5b01707
卷: 87, 期:17, 页:8789-8797
收录类别: SCI
文章类型: Article
WOS标题词: Science & Technology ;  Physical Sciences
类目[WOS]: Chemistry, Analytical
研究领域[WOS]: Chemistry
英文摘要: A 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.).
关键词[WOS]: POLYHEDRAL OLIGOMERIC SILSESQUIOXANE ;  RING-OPENING POLYMERIZATION ;  ENE CLICK CHEMISTRY ;  SMALL MOLECULES ;  STATIONARY PHASES ;  REVERSED-PHASE ;  SEPARATION ;  ELECTROCHROMATOGRAPHY ;  FUNCTIONALIZATION ;  MORPHOLOGY
语种: 英语
WOS记录号: WOS:000360773100029
Citation statistics: 
内容类型: 期刊论文
URI标识: http://cas-ir.dicp.ac.cn/handle/321008/146528
Appears in Collections:中国科学院大连化学物理研究所_期刊论文

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作者单位: 1.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:
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.
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