期刊
MICROCHEMICAL JOURNAL
卷 161, 期 -, 页码 -出版社
ELSEVIER
DOI: 10.1016/j.microc.2020.105783
关键词
Capillary electrochromatography; Liquid chromatography; Monolithic stationary phase; [3-(Methacryloxy)propyl]trimethoxysilane; Solid-state nuclear magnetic resonance; Capacitively coupled contactless conductivity detector
资金
- Conselho Nacional de Desenvolvimento Cientifico e tecnologico [CNPq - 303355/2017-4, 424032/20180, 304415/2013-8]
- INCTBio (FAPESP) [2014/50867-3]
- CNPq [465389/2014-7]
- Fundacao de Amparo a Pesquisa do Estado de Minas Gerais (FAPEMIG
- Rede Mineria de Quimica (RQ-MG) [CEX. RED-00010-14]
- Coordenacao de Aperfeicoamento de Pessoal de Nivel Superior [CAPES: PNPD 23071022702/2018-43, PDSE 88881187078/2018-01]
This study prepared monolithic stationary phases for capillary chromatography by polymerizing MPTMS monomer, applied them in separating PAHs, and attempted to improve the stationary phase by incorporating BM as a comonomer. The physical homogeneity of the columns was evaluated using an optical microscope and a conductivity detector, while the chemical characterization was done using solid-state NMR spectroscopy.
This work describes the preparation, characterization and application of monolithic stationary phases for capillary-scale chromatography. The columns were prepared by polymerization of [3-(methacryloxy)propyl] trimethoxysilane (MPTMS) monomer in two consecutive steps: i) sol-gel process and ii) photoinitiated radical addition. The photopolymerization was carried out in 100 um i.d. UV-transparent coating fused silica capillaries. The columns were applied in the qualitative separation of five polycyclic aromatic hydrocarbons (PAH) by both capillary liquid chromatography (nano-LC) and capillary electrochromatography (CEC) in a capillary electrophoresis equipment. In an attempt to improve the separation of the PAHs, the stationary phase was modified by incorporating benzyl methacrylate (BM) as a comonomer in the MPTMS-based polymer structure, but no improvement was observed. The physical homogeneity of the columns was evaluated by using an optical microscope and a capacitively coupled contactless conductivity detector ((CD)-D-4) as a non-invasive scanner moving longitudinally along the capillary. The chemical characterization of the polymer was done by both C-13 and Si-29 solid-state nuclear magnetic resonance spectroscopy (SSNMR). It was possible to propose a carbon chain structure and the substitution degree of the silyl group indicating the cross-linking of the polymer chains through the formation of dimers and trimers by condensation of the alkoxysilane groups.
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