Hybrid organic-inorganic phenyl monolithic column for capillary electrochromatography

A novel hybrid organic-inorganic silica-based monolithic column possessing phenyl ligands for reversed-phase (RP) capillary electrochromatography (CEC) is described. The monolithic stationary phase was prepared by in situ co-condensation of tetraethoxysilane (TEOS) with phenyltriethoxysilane (PTES) via a two-step catalytic sol-gel procedure to introduce phenyl groups distributed throughout the silica matrix for chromatographic interaction. The hydrolysis and condensation reactions of precursors were chemically controlled through pH variation by adding hydrochloric acid and dodecylamine, respectively. The structural property of the monolithic column can be easily tailored through adjusting the composition of starting sol solution. The effect of PTES/TEOS ratios on the morphology of the created stationary phases was investigated. A variety of neutral and basic analytes were used to evaluate the column performance. The CEC columns exhibited typical RP chromatographic retention mechanism for neutral compounds and had improved peak shape for basic solutes.

Preparation of monolithic silica column with strong cation-exchange stationary phase for capillary electrochromatography

A monolithic silica based strong cation-exchange stationary phase was successfully prepared for capillary electrochromatography. The monolithic silica matrix from a sol-gel process was chemically modified by treatment with 3-mercaptopropyltrimethoxysilane followed by a chemical oxidation procedure to produce the desired function. The strong cation-exchange stationary phase was characterized by its substantial and stable electroosmotic flow (EOF), and it was observed that the EOF value of the prepared column remained almost unchanged at different buffer pH values and slowly decreased with increasing phosphate concentration in the mobile phase. The monolithic silica column with strong cation-exchange stationary phase has been successfully employed in the electrochromatographic separation of beta-blockers and alkaloids extracted from traditional Chinese medicines (TCMs). The column efficiencies for the tested beta-blockers varied from 210,000 to 340,000 plates/m. A peak compression effect was observed for atenolol with the mobile phase having a low phosphate concentration.

Electrochromatographic evaluation of a silica monolith capillary column for separation of basic pharmaceuticals

A silica-based monolithic capillary column was prepared via a sol-gel process. The continuous skeleton and large through-pore structure were characterized by scanning electron microscopy (SEM). The native silica monolith has been successfully employed in the electrochromatographic separation of beta-blockers and alkaloids extracted from traditional Chinese medicines (TCMs). Column efficiencies greater than 250000 plates/m for capillary electrochromatography (CEC) separation of basic compounds were obtained. It was observed that retention of basic pharmaceuticals on the silica monolith was mainly contributed by a cation-exchange mechanism. Other retention mechanisms including reversed-phase and normal-phase mechanisms and electrophoresis of basic compounds also played a role in separation. A comparison of the differences between CEC and capillary zone electrophoresis (CZE) separation was also discussed.

Morphology transcription process from CMC micelles to inorganogel and its effect on the properties of alumina particle

In this study, a carboxymethyl cellulose (CMC)-mediated sol-gel process was developed to synthesize the alumina hydoxide whiskers. During the process, inexpensive inorganic salts were used as precursors and supercritical drying method was used to extract the water in hydrogel. The influences of CMC on the gel formation and the particle morphology were investigated. The results show that the formation of CMC-aluminium hydroxide organic-inorganic hybridgels led to a morphology transcription process from CMC micelles to aluminium hydroxide gel, as a result, the precursor with whiskerious morphology was obtained.

Post-grafting preparation of large-pore mesoporous materials with localized high content titanium doping

A new post-grafting process, consisting of two steps of substrate preparation and sol - gel post-grafting, has been developed to prepare titanium-doped mesoporous SBA-15 material with a double-layered structure and locally concentrated titanium content at the inner pore surface. With this novel technique, the single phased and originally ordered mesostructures can be well conserved; in the conventional direct synthesis they can be partially damaged when the frameworks are doped with high content heteroatoms. Titanium species exist in an isolated, tetrahedral structure and are localized at the pore surface; this is beneficial to both reactant access and product release. Characterization with XRD, N-2 adsorption/desorption isotherms, HREM/ EDS, ICP, UV - Vis, and the newly developed UV - Raman spectroscopy confirm these results. Preliminary catalytic tests with the selective epoxidation of cyclohexene show good catalytic activity. Among them, sample TiSBA-15-10 with a Si : Ti molar ratio of 10 shows a TON value of 75 and a highest product ( epoxide) yield of 55%.

Determination of organophosphorus pesticides in cucumber and potato by stir bar sorptive extraction

Organophosphorus pesticides (OPPs) in vegetables were determined by stir bar sorptive extraction (SBSE) and capillary gas chromatography with thermionic specific detection (TSD). Hydroxy-terminated polydimethylsioxane (PDMS) prepared by sol-gel method was used as extraction phase. The effects of extraction temperature, salting out, extraction time on extraction efficiency were studied. The detection limits of OPPs in water were <= 1.2 ng/l. This method was also applied to the analysis of OPPs in vegetable samples and matrix effect was studied. Linear ranges of OPPs in vegetable samples were 0.05-50 ng/g with detection limits <= 0. 15 ng/g and the repeatability of the method was less than 20% relative standard deviation. (c) 2005 Elsevier B.V. All rights reserved.