期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1379, 期 -, 页码 34-42出版社
ELSEVIER
DOI: 10.1016/j.chroma.2014.12.031
关键词
Polyhedral oligomeric silsesquioxane (POSS); Hybrid monolith; Thiol-methacrylate Michael addition reaction; Click chemistry; Capillary liquid chromatography
资金
- China State Key Basic Research Program [2013CB-911203, 2012CB910601]
- MOST [2012IM030400]
- National Natural Sciences Foundation of China [21235006, 21175133]
- NSFC [21321064]
- Knowledge Innovation program of DICP
- Dalian Institute of Chemical Physics of Chinese Academy of Sciences
A facile approach based on thiol-methacrylate Michael addition click reaction was developed for construction of porous hybrid monolithic materials. Three hybrid monoliths were prepared via thiol-methacrylate click polymerization by using methacrylate-polyhedral oligomeric silsesquioxane (POSS) (cage mixture, n = 8, 10, 12, POSS-MA) and three multi-thiol crosslinkers, 1,6-hexanedithiol (HDT), trimethylolpropane tris(3-mercaptopropionate) (TPTM) and pentaerythritol tetrakis(3-mercaptopropionate) (PTM), respectively, in the presence of porogenic solvents (n-propanol and PEG 200) and a catalyst (dimethylphenylphosphine, DMPP). The obtained monoliths possessed high thermal and chemical stabilities. Besides, they all exhibited high column efficiencies and excellent separation abilities in capillary liquid chromatography (cLC). The highest column efficiency could reach ca. 195,000 N/m for butylbenzene on the monolith prepared with POSS-MA and TPTM (monolith POSS-TPTM) in reversed-phase (RP) mode at 0.64 mm/s. Good chromatographic performance were all achieved in the separations of polycyclic aromatic hydrocarbons (PAHs), phenols, anilines, EPA 610 as well as bovine serum albumin (BSA) digest. The high column efficiencies in the range of 51,400-117,000 N/m (achieved on the monolith POSS-PTM in RP mode) convincingly demonstrated the high separation abilities of these thiol-methacrylate based hybrid monoliths. All the results demonstrated the feasibility of the phosphines catalyzed thiol-methacrylate Michael addition click reaction in fabrication of monolithic columns with high efficiency for cLC applications. (C) 2014 Elsevier B.V. All rights reserved.
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