Synthesis of spherical porous silicas in the micron and submicron size range: challenges and opportunities for miniaturized high-resolution chromatographic and electrokinetic separations

Unger, Klaus K.; Kumar, Dhananjay; Grün, M.; Büchel, Gunter; Lüdtke, Silke; Adam, Th.; Schumacher, Kai; Renker, Sabine

doi:10.1016/s0021-9673(00)00177-1

Cited by 179 publications

(103 citation statements)

References 13 publications

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“…Assim, após sua remoção por calcinação, a partícula de sílica apresenta maior porosidade. Unger et al [27] realizaram trabalhos empregando alquilaminas (dodecilamina e hexadecilamina) para produzir poros nas partículas de sílica sintetizadas pelo método de Stöber modificado. Similarmente, outros trabalhos têm mostrado bons resultados ao utilizar cloreto de hexadeciltrimetilamônio (CTAC) [28] ou brometo de hexadeciltrimetilamônio (CTAB) [29] como surfactante porogênico.…”

Section: O Processo Sol-gelunclassified

Suportes cromatográficos e fases estacionárias para cromatografia líquida: preparo, evolução e tendências

Nazário¹,

Lanças²

2013

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ResumoDesde o surgimento da instrumentação dedicada à HPLC, essa técnica analítica tem se destacado na separação e análise de uma grande variedade de compostos em diferentes campos de atuação. Nesse contexto, a área de pesquisa e desenvolvimento (P&D) de suportes cromatográficos e de fases estacionárias para HPLC tem recebido atenção de pesquisadores, objetivando análises rápidas, colunas eficientes e seletividade adequada. Neste trabalho discutem-se os métodos utilizados no preparo de suportes cromatográficos para HPLC (principalmente os baseados em sílica) e as estratégias de modificação de sua superfície no preparo de fases estacionárias. Palavras-chaveHPLC; suporte cromatográfico; sílica; fase estacionária.Chromatographic supports and stationary phases for liquid chromatography: preparation, evolution and trends AbstractSince the development of instrumentation for HPLC, this analytical technique has been widely employed in the separations and analysis of a large variety of compounds in different fields. In this context, research and development (R & D) area of chromatographic supports and stationary phases for HPLC have been receiving attention from researchers aiming the decrease in analysis time, increase column efficient and promote adequate selectivity. In this paper, we focused on the methods for the preparation of chromatographic supports for HPLC (especially silica-based materials) and strategies for modifying its surface in the preparation of stationary phases.

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Section: O Processo Sol-gelunclassified

Suportes cromatográficos e fases estacionárias para cromatografia líquida: preparo, evolução e tendências

Nazário¹,

Lanças²

2013

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“…1 There have been more review articles on various silica particles. A couple of reviews on most recent core-shell and very fine particles were presented in 2012 2 and 2011.…”

Section: Introductionmentioning

confidence: 99%

Porous Silica Particles As Chromatographic Separation Media: A Review

Cheong¹

2014

Bulletin of the Korean Chemical Society

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Porous silica particles are the most prevailing raw material for stationary phases of liquid chromatography. During a long period of time, various methodologies for production of porous silica particles have been proposed, such as crashing and sieving of xerogel, traditional dry or wet process preparation of conventional spherical particles, preparation of hierarchical mesoporous particles by template-mediated pore formation, repeated formation of a thin layer of porous silica upon nonporous silica core (core-shell particles), and formation of specific silica monolith followed by grinding and calcination. Recent developments and applications of useful porous silica particles will be covered in this review. Discussion on sub-3 µm silica particles including nonporous silica particles, carbon or metal oxide clad silica particles, and molecularly imprinted silica particles, will also be included. Next, the individual preparation methods and their feasibilities will be collectively and critically compared and evaluated, being followed by conclusive remarks and future perspectives.

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“…These studies found that the phase ratio and capacity for nonporous submicron particles are very low and that high pressures made preparation of the capillary columns difficult [21][22][23][24][25]. The earliest work on the application of submicron silica particles in CEC was reported by Unger et al [26]. They focused on the preparation of submicron spherical silica particles by tailoring MCM-41S materials for separation applications using long-chain alkyltrimethoxysilane or alkylamines as porogens and achieved fast separation of mixtures of parabenes and polyaromatic compounds [27].…”

Section: Introductionmentioning

confidence: 99%

“…They compared the EOF of 0.2, 0.5, 1 and 3 mm porous silica particles and concluded that submicron silica particles were also able to generate EOF for CEC [28]. The use of submicron silica particles and their limits in HPLC, CE and CEC has also been summarized in Unger's review article [29] By contrast, there are few reports of CEC enantioseparation with small particle silica-packed columns. The most relevant work was done by Okamoto et al in which 1100 nm magnetic polymer particles functionalized with avidin were packed by magnetic field and used for enantioseparation of ketoprofen [30].…”

Section: Introductionmentioning

confidence: 99%

Monodispersed submicron porous silica particles functionalized with CD derivatives for chiral CEC

Wang

Young

et al. 2010

Electrophoresis

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Rapid and efficient enantioseparation of halogen aryl alcohols and beta-blockers propranolol and pindolol in packed bed CEC (p-CEC) using as-prepared submicron porous silica chiral stationary phases (CSPs) has been achieved. Monodispersed 0.66 and 0.81 microm chiral submicron porous silica spheres were prepared using tetramethoxysilane and hexadecyltrimethylammonium bromide, followed by a hydrothermal treatment method with ammonia-ethanol to expand the pore of silica spheres without changing their spherical morphology. A proper specific surface of ca. 230 m(2)/g and pore sizes average of 6-8 nm were obtained by this method. The submicron porous silica spheres were modified with mono-6-phenylcarbamoylated beta-CD via thiol-en radical addition. They were packed into 9 cm 50 microm id capillary columns with photopolymerized monolithic frits. These submicron CSPs showed greater column efficiency (about 476 000 plates/m for 4-iodophenyl-1-ethanol) and higher resolution than the corresponding 3 microm CSP.

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Synthesis of spherical porous silicas in the micron and submicron size range: challenges and opportunities for miniaturized high-resolution chromatographic and electrokinetic separations

Cited by 179 publications

References 13 publications

Suportes cromatográficos e fases estacionárias para cromatografia líquida: preparo, evolução e tendências

Suportes cromatográficos e fases estacionárias para cromatografia líquida: preparo, evolução e tendências

Porous Silica Particles As Chromatographic Separation Media: A Review

Monodispersed submicron porous silica particles functionalized with CD derivatives for chiral CEC

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