[3-(Methacryloxy)propyl]trimethoxysilane-based monolithic stationary phases for capillary-scale chromatography and their characterization by contactless conductivity detection and solid-state NMR spectroscopy

Autor(es)

Marques, Rafael ^[1] ; Lima, Nerilson M. ^[1] ; Cantarino, Luiz Felipe ^[1] ; de Carvalho, Gustavo S. G. ^[1] ; Leitao, Alexandre A. ^[1] ; do Lago, Claudimir Lucio ^[2] ; de Oliveira, Marcone A. L. ^[1]

Afiliação do(s) autor(es)

^[1] Univ Fed Juiz de Fora, Inst Ciencias Exatas, Dept Quim, BR-36036900 Juiz de Fora, MG - Brazil

^[2] Univ Sao Paulo, Dept Quim Fundamental, Inst Quim, Av Prof Lineu Prestes 748, BR-05508900 Sao Paulo, SP - Brazil

• Tipo de documento: Artigo Científico
• Fonte: Microchemical Journal; v. 161, FEB 2021.
• Citações Web of Science: 0

Resumo

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. (AU)

• Processo FAPESP: 14/50867-3 - INCT 2014: Instituto Nacional de Ciência e Tecnologia de Bioanalítica
• Beneficiário: Marco Aurelio Zezzi Arruda
• Modalidade de apoio: Auxílio à Pesquisa - Temático