Article

Synthesis of sulfo/vinyl biphasic silica hybrid monolithic capillary column and its application to on-column preconcentration for capillary electrochromatography.

State Key Laboratory of Chemo/Biosensing & Chemometrics, College of Chemistry & Chemical Engineering, Hunan University, Changsha 410082, China.
Journal of Chromatography A (Impact Factor: 4.61). 01/2012; 1233:91-9. DOI: 10.1016/j.chroma.2012.01.024
Source: PubMed

ABSTRACT A novel method to synthesize sulfo/vinyl biphasic silica hybrid monolithic column in one step was developed for on-column preconcentration. In this method, sulfo-based segment is located at the inlet of capillary column, which acts as preconcentration column. It is synthesized by polymerization of 3-sulfopropyl methacrylate potassium salt (SPMA) and vinyltrimethoxysilane (VTMS) with tetramethoxysilane (TOMS). Close to the preconcentration column, a vinyl functionalized segment is formed and serves as separation column. It is synthesized by polymerization of only VTMS with TOMS. Vinyl groups on vinyl functionalized segment are modified with ligand containing sulfhydryl group, such as octadecanethiol (C(18)-SH for short), 6-mercapto-1-hexanol (HO-C(6)-SH for short), via thiol-ene click reaction. The interface between the two segments is seamless and without any dead volume. The applicability of this system is demonstrated by successful separation of closely related amines including p-phenylenediamine, aniline, p-toluidine, N-methyl aniline, N,N'-dimethylaniline, and diphenylamine. Good separation and enrichment are obtained. The proposed system is also successfully applied to complex biological samples, such as peptide, diluted BSA hydrolysate, and the results indicate that the system has a capability for preconcentration of low abundance peptides.

0 Bookmarks
 · 
72 Views
  • [Show abstract] [Hide abstract]
    ABSTRACT: A novel (3-sulfopropyl methacrylate potassium)-silica hybrid monolithic column for capillary electrochromatography (CEC) has been prepared by a simple one-pot approach based on efficient thiol-ene click chemistry. In this process, the polycondensation of hydrolyzed alkoxysilanes and in situ click reaction of vinyl groups on 3-sulfopropyl methacrylate potassium (SPMA) and thiol groups on the precondensed siloxanes simultaneously occured in a pretreated capillary. Homogeneous monolithic matrix with large through-pores tightly bonded to the inner wall of the capillary was shown by optical microscope and scanning electron microscope (SEM). The minimum plate height of this hybrid monolithic column was determined as 3.9 μm for thiourea. Anilines, alkylbenzenes and phenols were well separated on this hybrid monolithic column by CEC, which indicated typical reversed-phase and cation-exchange chromatographic retention mechanisms of the column.
    Electrophoresis 11/2012; · 3.26 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: Trends in Liquid Chromatography focuses on dedicated separation developments spanning different field of application ranging from sample preparation issues to miniaturization purposes. Chromatographic performances result from the porous media, its implantation inside "column" and its surface functionalization. Because molecular interactions govern chromatographic phenomena, surface functionalization is still a hot research topic. Besides standard approaches leading to surface functionalization, the use of new surface chemistry reactions opens new perspectives. Click chemistry belongs to this new class of chemical reactions, characterized by their specificity, compatibility with aqueous media and high reaction yields. In this frame, we review the use of click chemistry reactions in chromatographic sciences. In a first part, we present the click chemistry with a specific focus on its implementation in stationary phases. The use of these new clicked materials is detailed and discussed with respect to the chromatographic mode. This article is protected by copyright. All rights reserved.
    Journal of Separation Science 04/2013; · 2.59 Impact Factor
  • [Show abstract] [Hide abstract]
    ABSTRACT: A porous monolith was prepared by in situ free-radical polymerization using N-isopropylacrylamide (NIPAAm) and trimethylol propane triacrylate (TMPTA) as functional monomers, ethylene dimethacrylate (EDMA) as crosslinking agent. The chemical group of the monolith was assayed by a Fourier transform infrared spectroscopy (FT-IR) method and the morphology of optimized monolithic column was characterized by scanning electron microscopy (SEM). The mechanical strength and permeability have been studied in detail as well. The run-to-run and column-to-column reproducibility of the retention times were less than 0.9% and 3.0%, respectively. Furthermore, the influence of temperature and mobile phase composition on the separation of aromatic compounds was investigated. The results indicated that poly (trimethylol propane triacrylate-co-N-isopropylacrylamide-co-ethylenedimethacrylate) (TMPTA-co-NIPAAm-co-EDMA) monolithic column not only had high porosity and strong rigidity, but also was a promising tool for analyzing small molecule compounds with a short analysis time by controlling the column temperature.
    Journal of Chromatography A 11/2013; · 4.61 Impact Factor