Hydrophobic sol-gel channel patterning strategies for paper-based microfluidics.

Hydrophobic sol-gel derived methylsilsesquioxane (MSQ) was compared to wax and alkylketene dimer (AKD) as barrier materials defining channels in paper-based microfluidic devices. While all three of the barrier types performed well with water, only the MSQ barriers were not breached by aggressive cell lysing solutions and surfactant solutions (SDS, CTAB, Triton X-100). The MSQ barriers also withstood glycerol, toluene and DMSO whereas all three barrier types were breached by alcohols.

Thin-film octadecyl-silica glass coating for automated 96-blade solid-phase microextraction coupled with liquid chromatography-tandem mass spectrometry for analysis of benzodiazepines.

A thin-film octadecyl (C18)-silica glass coating was developed as the extraction phase for an automated 96-blade solid-phase microextraction (SPME) system coupled with liquid chromatography-tandem mass spectrometry (LC-MS/MS). Various factors (e.g.

A sol-gel-derived acetylcholinesterase microarray for nanovolume small-molecule screening.

A fluorimetric acetylcholinesterase (AChE) assay was developed and characterized both in solution and with the enzyme entrapped in sol-gel-derived silica. The assay is based on a disulfide-thiol interchange reaction between the intramolecularly quenched dimeric dye BODIPY FL l-cystine and thiocholine generated by the AChE-catalyzed hydrolysis of acetylthiocholine (ATCh), which results in a brightly fluorescent monomeric product owing to the cleavage of the disulfide-coupled form of the dye. The new assay was validated by comparison with the Ellman assay performed under parallel conditions and was used in both kinetic and end point assays.

Silicate-entrapped porous coatings for preparing high-efficiency solid-phase microextraction sorbents.

We present a novel way to prepare SPME fibers using a silicate entrapment of porous particles, followed by derivatization using classical organosilane chemistry. The fibers provide a good platform for on-fiber derivatization of desired extraction phases while providing porosity necessary for high extractions capacities. The porous network was created using potassium silicate and porous silica particles.

Polymer entrapment in polymerized silicate for preparing highly stable capillary coatings for CE and CE-MS.

An easy-to-implement capillary coating strategy based on polymer entrapment in the network of polymerized silicate is described. In this manner, cationic polymers are tightly fixed onto the inner wall of the capillary for electroosmotic flow control without necessitating complex surface modification chemistries. The resulting coated capillary exhibited good stability over a wide range of pH, good reproducibility, strong endurance in more than 300 electrophoretic runs, and tolerance of commonly employed organic solvent additives in CE.

Simple on-line sample preconcentration technique for peptides based on dynamic pH junction in capillary electrophoresis-mass spectrometry.

We report an on-line sample preconcentration technique based on dynamic pH junction in capillary electrophoresis-mass spectrometry (CE-MS). For peptide analysis, the samples were dissolved in a solution with higher pH than the background solution (BGS), and were injected into the capillary as a long plug. The pH difference between the sample matrix and BGS caused changes in analytes' mobilities during electrophoresis, resulting in narrowing of their bands at the boundary.

Metabolome analysis by capillary electrophoresis-mass spectrometry.

Capillary electrophoresis (CE)-mass spectrometry (MS), as an analytical platform, has made significant contributions in advancing metabolomics research, if still limited up to this time. This review, covering reports published between 1998 and 2006, describes how CE-MS has been used thus far in this field, with the majority of the works dealing with targeted metabolite analyses and only a small fraction using it in the comprehensive context. It also discusses how some of the key features of CE-MS were exploited in selected metabolomic applications.

Sample enrichment techniques in capillary electrophoresis: focus on peptides and proteins.

Compared to chromatography-based techniques, the concentration limits of detection (CLOD) associated with capillary electrophoresis are worse, and these have largely precluded their use in many practical applications. To overcome this limitation, researchers from various disciplines have exerted tremendous efforts toward developing strategies for increasing the concentration sensitivities of capillary electrophoresis (CE) systems, via the so-called sample enrichment techniques. This review highlights selected developments and advances in this area as applied to the analyses of proteins and peptides in the last 5 years.

Dynamic pH junction technique for on-line preconcentration of peptides in capillary electrophoresis.

A method based on the presence of a dynamic pH junction within the capillary to induce band narrowing for enhanced detection sensitivity for some peptides is presented. This technique is predicated on a sharp reduction in an analyte's migration velocity following a reversal of its electrophoretic direction from the acidic sample zone to the basic BGS zone. Larger-than-usual injection volumes of samples in relatively high-conductivity matrices were enabled, without degrading peak shape, resolution and efficiency.

Recent developments in capillary electrophoresis-mass spectrometry of proteins and peptides.

Many researchers have invested considerable efforts toward improving capillary electrophoresis (CE)-mass spectrometry (MS) systems so they can be applied better to standard analyses. This review highlights the developments in CE-MS of proteins and peptides over the last five years. It includes the developments in interfaces, sample-enrichment techniques, microfabricated devices, and some applications, largely in capillary zone electrophoresis (CZE), capillary isoelectric focusing (CIEF) and capillary isotachophoresis formats.

Field-enhanced sample injection for high-sensitivity analysis of peptides and proteins in capillary electrophoresis-mass spectrometry.

Field-enhanced sample injection (FESI) was used to improve the concentration sensitivity of a capillary electrophoresis (CE)-mass spectrometry (MS) system with sheath flow configuration. Using some bioactive peptides, more than 3000-fold improvement in signal was obtained, permitting analysis in the low nM (fmol/microl) levels. The system was further evaluated for analysis of complex peptide mixtures by using low concentration tryptic digests of standard proteins.

On-line sample preconcentration in micellar electrokinetic chromatography by sweeping with anionic-zwitterionic mixed micelles.

On-line preconcentration by sweeping in micellar electrokinetic chromatography using mixed micelles of sodium dodecyl sulfate (SDS)-SB-12 is presented. Because of their large micelle radius, they permit increased partitioning of hydrophobic analytes into the core. In addition, they also possess lower negative surface charge relative to pure SDS micelles so anionic analytes can be retained better due to decreased electrostatic repulsion.