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Preparation of open tubular capillary columns by in situ ring-opening polymerization and their applications in cLC-MS/MS analysis of tryptic digest

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Indexed by:期刊论文

Date of Publication:2017-08-01

Journal:ANALYTICA CHIMICA ACTA

Included Journals:SCIE、EI、PubMed、Scopus

Volume:979

Page Number:58-65

ISSN No.:0003-2670

Key Words:Open tubular column; Octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxanes; 4-aminophenyl disulfide; Ring-opening polymerization; Capillary liquid chromatography

Abstract:An open tubular (OT) column (25 mu m i.d.) was prepared by in situ ring-opening polymerization of octaglycidyldimethylsilyl polyhedral oligomeric silsesquioxanes (POSS-epoxy) with 4-aminophenyl di-sulfide (APDS) in a binary porogenic system of ethanol/H2O. It was found that porogenic composition played an important role in the formation of OT stationary phases. The ratio of ethanol/H2O at 6/1 (v/v) would lead to the fabrication of hybrid monoliths, while the ratio of ethanol/H2O at 13/1 (v/v) would result in the synthesis of OT phases. In addition, the effects of precursor content and reaction duration on the thickness of OT stationary phases were investigated. Either lower precursor content or shorter reaction duration would produce thinner layer of OT column. The repeatability of OT columns was evaluated through relative standard deviation (RSD%) with benzene as the analyte. The run-to-run, columnto- column and batch-to-batch repeatabilities were 1.7%, 4.8% and 5.6%, respectively, exhibiting satisfactory repeatability of the OT column. Then tryptic digest of mouse liver proteins was used to evaluate the performance of the resulting OT columns (25 mu m i.d. x 2.5 m in length) by cLC-MS/MS analysis, demonstrating their potential in proteome analysis. (C) 2017 Elsevier B.V. All rights reserved.

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