Energy-efficient and environment-friendly method to prepare monodispersed silica stationary phases for simultaneous separation of compound drugs.

An energy-efficient and environment-friendly approach to prepare porous monodispersed micro-sized silica particles with methyltrimethoxysilane (MTMS) as the precursor is described. The particles were synthesized by a two-step hydrolysis/condensation procedure, with post-synthetic aging and calcination for methyl group removal. They show uniform spherical morphology, narrow particle size distribution (D/, 1.

Inverse Mixed-Mode Chromatography for the Evaluation of Multivalency and Cooperativity of Host-Guest Complexation in Porous Materials.

A new separation-based analytical method was developed to evaluate the multivalency and cooperativity of supramolecular host-guest complexation in porous materials. The method is based on inverse mixed-mode chromatography in which a porous material with a multivalent functional group is packed into a column and bound with a complementary guest molecule to form a multivalent complex. The bound guest molecules are eluted in the mobile phase and detected by appropriate methods such as UV absorption.

Epoxide-derived mixed-mode chromatographic stationary phases for separation of active substances in fixed-dose combination drugs.

A method for the preparation of novel mixed-mode reversed-phase/strong cation exchange stationary phase for the separation of fixed-dose combination drugs has been developed. An epoxysilane bonded silica prepared by vapor phase deposition was used as a starting material to produce diol, octadecyl, sulfonate, and mixed octadecyl/sulfonate groups bonded silica phases. The chemical structure and surface coverage of the functional groups on these synthesized phases were confirmed by fourier-transform infrared and solid-state C NMR spectroscopy and elemental analysis.

Synthesis and evaluation of porous polymethylsilsesquioxane microspheres as low silanol activity chromatographic stationary phase for basic compound separation.

Polymethylsilsesquioxanes (PMSQ) are potentially useful materials for liquid chromatography owing to their unique chemical, electrical and mechanical properties. Surprisingly however, no systematic studies on the use of spherical PMSQ particles as chromatographic packing have been reported. Accordingly, we present a comprehensive study aimed to characterize the chromatographic properties of this material in high performance liquid chromatography (HPLC) and to compare them with those observed on methyl (C) bonded silica phase under comparable conditions.

Separation and identification of oligomeric vinylmethoxysiloxanes by gradient elution chromatography coupled with electrospray ionization mass spectrometry.

A high-performance liquid chromatography with online electrospray ionization mass spectrometry (HPLC-ESI-MS) has been used to separate and identify the reaction products resulting from controlled acid-catalyzed hydrolytic polycondensation of vinyltrimethoxysilane (VMS). The reaction products were prepared in the molar ratio of water to VMS (r1) ranging from 0.6 to 1.

Separation and identification of oligomeric phenylethoxysiloxanols by liquid chromatography-electrospray ionization mass spectrometry.

Liquid chromatography-electrospray ionization mass spectrometry has been applied to qualitative analysis of oligomeric phenylethoxysiloxanols, a class of organosilanols as active intermediates to polyhedral silsesquioxanes. The phenylethoxysiloxanol samples were prepared by controlled acid-catalyzed hydrolysis and condensation of phenyltriethoxysilane at various molar equivalents of water (r1) and characterized by standard spectroscopic techniques. Using a gradient binary water-methanol mobile phase, these reaction products were resolved on octadecylsiloxane silica stationary phase and subsequently identified by online electrospray ionization mass spectrometric detection.

Separation and identification of oligomeric ethyl silicates by liquid chromatography with electrospray ionization mass spectrometry.

Reversed-phase liquid chromatography coupled with electrospray ionization mass spectrometry was used to study the molecular structures of components and molar mass distributions in ethyl silicate-40, a versatile liquid precursor for silicon-based materials. Identity testing by standard spectroscopic techniques showed that a commercial sample of ethyl silicate-40 was composed of linear/branched ethoxysiloxane oligomers with the silicon atoms ranging from 2 to 12 together with minor monocyclic species. Analysis of the sample by liquid chromatography coupled with evaporative light scattering detection resulted in an elution profile consisting of a series of peak clusters.

Separation and identification of an oligomeric light stabilizer Chimassorb 944 by gradient elution chromatography coupled with matrix-assisted laser desorption/ionization mass spectrometry.

A non-aqueous reversed-phase high-performance liquid chromatographic (HPLC) method has been developed to separate a light stabilizer Chimassorb 944 into individual oligomers, which are further identified using pre-column fluorescent derivatization and matrix-assisted laser desorption/ionization mass spectrometry (MALDI-MS). Consistent with previous studies, we find that the Chimassorb 944 product is a complex mixture consisting of a homologous series with the amine end groups and the number of repeat units (n) span from 1 to 26. In addition to the dominant linear species, cyclic oligomers are present at relatively high levels in the low-mass range.

Field-flow fractionation of magnetic particles in a cyclic magnetic field.

Although magnetic field-flow fractionation (MgFFF) is emerging as a promising technique for characterizing magnetic particles, it still suffers from limitations such as low separation efficiency due to irreversible adsorption of magnetic particles on separation channel. Here we report a novel approach based on the use of a cyclic magnetic field to overcome the particle entrapment in MgFFF. This cyclic field is generated by rotating a magnet on the top of the spiral separation channel so that magnetic and opposing gravitational forces alternately act on the magnetic particles suspended in the fluid flow.

Preparation of magnetite-loaded silica microspheres for solid-phase extraction of genomic DNA from soy-based foodstuffs.

Solid-phase extraction has been widely employed for the preparation of DNA templates for polymerase chain reaction (PCR)-based analytical methods. Among the variety of adsorbents studied, magnetically responsive silica particles are particularly attractive due to their potential to simplify, expedite, and automate the extraction process. Here we report a facile method for the preparation of such magnetic particles, which entails impregnation of porous silica microspheres with iron salts, followed by calcination and reduction treatments.

Magnetically immobilized frits for the preparation of packed columns used in capillary electrochromatography.

Fabrication of porous frits to retain stationary phases is a critical issue in column preparation for capillary electrochromatography (CEC). In this work, porous frits were prepared by applying an external magnetic field to magnetically responsive particles placed inside a fused-silica capillary. Three batches of uniform magnetite spheres with particle diameters of 0.

Magnetically immobilized beds for capillary electrochromatography.

Fritless packed beds comprised of magnetically responsive octadecylsilane bonded silica particles have been constructed for reversed-phase electrochromatography. The magnetic particles were immobilized in the capillary by applying an external magnetic field transverse to the direction of electroosmotic flow. Being subjected to the interplay of fluid dragging and magnetic forces, the initial loosely packed particle assembly was compacted into a uniform packing structure.

Synthesis of novel porous magnetic silica microspheres as adsorbents for isolation of genomic DNA.

An improved procedure is described for preparation of novel mesoporous microspheres consisting of magnetic nanoparticles homogeneously dispersed in a silica matrix. The method is based on a three-step process, involving (i) formation of hematite/silica composite microspheres by urea-formaldehyde polymerization, (ii) calcination of the composite particles to remove the organic constituents, and (iii) in situ transformation of the iron oxide in the composites by hydrogen reductive reaction. The as-synthesized magnetite/silica composite microspheres were nearly monodisperse, mesoporous, and magnetizable, with as typical values an average diameter of 3.

Packing structure and self-heating in capillary electrochromatography.

The origin of bubble formation during operation of capillary electrochromatography (CEC) has been an issue of debate. Ohmic heating resulted from current passed through a packed column was proposed as the primary cause. However, this explanation has been questioned on the ground that the current measured in CEC is much lower than that measured with open-tubular separation systems where no bubble formation occurs.

Measurement of packing tortuosity and porosity in capillary electrochromatography.

The application of conductivity measurements for packing structure characterization has been extended to a column consisting of a packed section and an open section as typically used in capillary electrochromatography (CEC). Because of the difference in electric conductivity between the packed and open sections, the electric fields applied across the two sections vary, depending on the length of the packed section relative to that of the total column. On the basis of mass conservation law, it can be shown that the ratio of the electric current measured in such a duplex column to that without packing is a function of the length and the geometric structure of the packing bed.

Fluorescence polarization detection for affinity capillary electrophoresis.

Affinity capillary electrophoresis (ACE) with laser-induced fluorescence polarization (LIFP) detection is described, with examples of affinity interaction studies. Because fluorescence polarization is sensitive to changes in the rotational motion arising from molecular association or dissociation, ACE-LIFP is capable of providing information on the formation of affinity complexes prior to or during CE separation. Unbound, small fluorescent probes generally have little fluorescence polarization because of rapid rotation of the molecule in solution.