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Biomedical subjects

Joseph J Pesek

Publications and source records attributed to Joseph J Pesek.

At least 19 recordsLinked to original sources
PubMed2006

Open tubular capillary electrochromatography migration behavior of enkephalins in etched chemically modified fused silica capillaries.

Fused silica capillaries for use in electrophoretic analyses are etched with ammonium bifluoride in the presence of a second inorganic salt (CuCl(2), CrCl(3), NaNO(3), or (NH(4))(2)CO(3)). The effects of the presence of these inorganic components in the surface matrix on the electromigration behavior of enkephalins are evaluated. Resolution, efficiency and peak shape are used to compare the various columns. In some cases the etched surface is then modified by the addition of an octadecyl moiety using a silanization/hydrosilation procedure. The surface properties of the etched capillaries can also be evaluated by electroosmotic flow measurements. RSDs of migration times under identical experimental conditions were <1%.

Chromatography, Micellar Electrokinetic Capillary↗
PubMed2006

Synthesis and HPLC evaluation of carboxylic acid phases on a hydride surface.

Three organic moieties containing carboxylic acid functional groups are attached to a particulate silica surface through silanization/hydrosilation. Two compounds (undecylenic acid and 10-undecynoic acid) have 11 carbon chains and the other is a five-carbon acid (pentenoic acid). Bonding is confirmed through carbon elemental analysis, diffuse reflectance infrared fourier transform spectroscopy, and carbon-13 and silicon-29 CP-MAS NMR spectroscopy. The bonded phases are tested by HPLC using PTH amino acids, nucleic acids, theophylline-related compounds, anilines, benzoic acid compounds, choline, and tobramycin. The latter two compounds are used to investigate the aqueous normal phase properties of the three bonded materials.

Amino Acids↗
PubMed2005

Comparison of silanization/hydrosilation and organosilanization modification procedures on etched capillaries for electrokinetic chromatography.

Etched capillaries for use in open tubular electrochromatography are modified by silanization/hydrosilation and organosilanization. The migration behavior of both types of capillaries is evaluated with small basic molecules, peptides and proteins. Comparisons of peak symmetry and efficiency are used to measure the effectiveness of the two methods for modifying the etched surface. From this information, the suitability of each method for use with etched capillaries can be determined.

Chromatography, Micellar Electrokinetic Capillary↗
PubMed2005

The use of etched, chemically modified, rectangular capillaries as a separation medium for open tubular capillary electrochromatography.

The use of etched, chemically modified, capillaries with a rectangular inner channel for open tubular electrochromatography is investigated. Comparisons of separation capabilities are made between circular and rectangular capillaries undergoing the same etching and chemical modification processes. With the long dimension of the rectangular column aligned in the direction of the optical light path, the relative sensitivities of the two capillary geometries are evaluated. The electrochromatographic properties of two catechins found in tea are investigated on the rectangular etched octadecyl-modified capillary.

Carbon↗
PubMed2005

Use of inorganic salts during the etching process in the fabrication of chemically modified capillaries for open tubular electrochromatography.

Capillaries for use in electrophoretic analyses are etched with ammonium bifluoride and in some cases a second inorganic salt is included in the process. The effects of the presence of these inorganic components in the surface matrix on the electromigration of heterocyclic aromatic amines and enkephalins are evaluated. Resolution, efficiency, and peak shape are used to compare the various columns. In one instance, the etched surface is then modified by the addition of an octadecyl moiety using a silanization/hydrosilation procedure. The surface properties of the various etched capillaries are also compared by electroosmotic flow measurements.

Alkenes↗
PubMed2005

Hydride-based silica stationary phases for HPLC: fundamental properties and applications.

Silica hydride is a recent development in chromatographic support materials for HPLC where hydride groups replace 95% of the silanols on the surface. This conversion changes many of the fundamental properties of the material as well as the bonded stationary phases that are the result of further chemical modification of the hydride surface. The general approach for fabricating the silica hydride and subsequent bonded phases is reviewed. Properties of the silica hydride surface are compared to those of the standard material obtained in the preparation of most commercial HPLC stationary phases. Some unique chromatographic properties of hydride-based phases are described as well as some general application areas where these bonded materials may be used in preference to or have advantages not available from typical stationary phases.

Chromatography, High Pressure Liquid↗
PubMed2005

Synthesis and characterization of chemically bonded stationary phases on hydride surfaces by hydrosilation of alkynes and dienes.

A hydrosilation reaction was used to bind four compounds with one or more alkyne groups or two alkene functionalities. The diffuse reflectance infrared Fourier transform, the 29Si cross-polarization magic-angle spinning (CP-MAS) NMR, and the 13C CP-MAS NMR spectra were used to characterize the various bonded materials. The bonded phase density was determined from carbon elemental analysis. The two ten-carbon hydrophobic stationary phases were characterized chromatographically and static stability tests were run in acidic and basic solutions.

Alkynes↗
PubMed2005

Hydride-based separation materials for high performance liquid chromatography and open tubular capillary electrochromatography.

Silica hydride is a recent development in chromatographic support materials for high performance liquid chromatography (HPLC) where hydride groups replace 95% of the silanols on the surface. This conversion changes many of the fundamental properties of the material as well as the bonded stationary phases that are the result of further chemical modification of the hydride surface. Some unique chromatographic properties of hydride-based phases are described as well as some general application areas where these bonded materials may be used in preference to or have advantages not available from typical stationary phases. The fabrication, properties and applications of etched chemically modified capillaries for electrophoretic analysis are also reviewed. It is shown that the etching process creates a surface that is fundamentally different than a bare fused silica capillary. The new surface matrix produces unique electroosmotic flow properties and is more compatible with basic and biological compounds. After chemical modification of the surface, the bonded organic moiety (stationary phase) contributes to the control of migration of solutes in the capillary. Both electrophoretic and chromatographic processes take place in the etched chemically modified capillaries leading to a variety of experimental variables that can be used to optimize separations. A number of examples of separations on these capillaries are described.

Capillary Electrochromatography↗
PubMed2004

Electrochromatographic studies of etched capillaries modified with a cyano pentoxy biphenyl liquid crystal.

A liquid crystal stationary phase for open tubular capillary electrochromatograpy (OTCEC) is fabricated by etching a fused silica tube and then bonding 4,4'-cyanopentoxy biphenyl by a silanization/hydrosilation process. The versatility of this electrophoretic capillary is demonstrated by separations of proteins, peptides, basic pharmaceuticals and the metabolites of tryptophan. Chromatographic interactions are verified by resolution of two neutral peptides. Variable temperature studies are used to understand the liquid crystal properties of the bonded moiety. EOF measurements as a function of pH and temperature further characterize this unique separation media.

Chromatography, Micellar Electrokinetic Capillary↗
PubMed2004

Separation of polyethylene glycol-modified proteins by open tubular capillary electrochromatography.

This study involves the characterization of six polyethylene glycol-modified proteins by open tubular capillary electrochromatography, a high-resolution, versatile and reproducible technique for the analysis of biomolecules and pharmaceuticals. Optimized conditions were obtained with respect to type of capillary modification (cholesterol and octadecyl), applied voltage (+20 and -20 kV), buffer pH (2.14-8.14) and addition of methanol modifier to the mobile phase. Electrochromatograms were obtained with both cathodic and anodic applied electric fields. In the case of one PEG-protein, superoxide dismutase, a comparison was made to a previous study. Reproducibility and column lifetime were also evaluated in assessing the usefulness of the method.

Chromatography, Micellar Electrokinetic Capillary↗
PubMed2004

Open tubular capillary electrochromatography of synthetic peptides on etched chemically modified columns.

Two sets of peptides, each having structurally similar amino acid sequences, have been investigated by capillary electrochromatography (CEC) using etched chemically modified capillaries as the separation medium. In comparison to gradient RP-HPLC, the resolving power of the described CEC methods has been found to be superior. A number of variables have been examined with respect to optimization of the separation of these closely related peptides with several different etched chemically modified capillaries. These experimental variables included the nature of the bonded moiety, the pH, the organic modifier type, and the amount of organic modifier in the buffer electrolyte. Systematic variation of these parameters results in significant changes in the migrational behavior of the investigated peptides and provides important insight into the underlying molecular separation processes that prevail in open tubular CEC. Moreover, under optimized conditions, efficient separations characterized by highly symmetrical peaks were achieved. In addition, this study has permitted the long-term stability as well as the short-term and long-term reproducibility of the etched chemically modified capillaries to be documented.

Amino Acid Sequence↗
PubMed2004

Open-tubular electrochromatographic characterization of synthetic peptides.

The open-tubular electrochromatographic (OT-CEC) migration behavior of a series of peptides, based on a common structural feature, has been characterized using two different types of chemically modified etched capillaries. The organic moieties immobilized onto the capillary inner surface were n-butylphenyl and cholesterol-10-undecenaoate, respectively. The structure-migration behavior of this set of peptides has been studied at several pH values and with methanol at different concentrations as an organic solvent modifier of the buffer electrolyte composition. By comparing the structural properties of the peptides, such as their amino acid sequences, charge-to-mass ratios and intrinsic hydrophobicities to their migrational behavior, the relative contribution of electrophoretic and chromatographic mobility to the overall migration times, elution order, and selectivity has been determined. Moreover, the experimental data provide important insight into procedures that can be used to modulate the separation of peptides in OT-CEC through variation of the composition of the electrolyte buffer as well as via the properties of the bonded organic moiety.

Amino Acid Sequence↗
PubMed2004

Etched chemically modified capillaries: novel separation media for electrophoretic analyses.

The fabrication, properties, and applications of etched chemically modified capillaries for electrophoretic analysis are reviewed. It is shown that the etching process creates a surface that is fundamentally different than a bare fused silica capillary. The new surface matrix produces unique electroosmotic flow properties and is more compatible with basic and biological compounds. After chemical modification of the surface, the bonded organic moiety (stationary phase) contributes to the control of migration of solutes in the capillary. Both electrophoretic and chromatographic processes take place in the etched chemically modified capillaries leading to a variety of experimental variables (pH, buffer type, presence and amount of organic modifier, and temperature) that can be used to optimize separations. A number of examples of separations on these capillaries are presented as well as data on column ruggedness and reproducibility.

Buffers↗
PubMed2003

Synthesis and evaluation of a C8 stationary phase on a silica hydride surface by hydrosilation of 1-octyne.

The silanization/hydrosilation method is used to bond an alkyne (1-octyne) to a silica hydride surface. The new bonded material is characterized by elemental analysis and diffuse reflectance infrared Fourier transform spectroscopy. The hydrophobic behavior of this material was determined by the retention characteristics of aromatic solutes and the shape selectivity as well as phase classification (monomeric or polymeric) was measured by the polycyclic aromatic hydrocarbon mixture standard reference material 869. The presence of residual silanols on the bonded phase was probed by several basic solutes at pH 7. Long-term stability studies were conducted by measuring retention and peak symmetry of basic compounds over several thousand column volumes at pH 10.

Alkynes↗
PubMed2003

Cholesterol bonded phase as a separation medium in liquid chromatography. Evaluation of properties and applications.

An extensive survey of the properties and separation capabilities of a cholesterol bonded phase is reported. The intermediate hydrophobic/hydrophilic properties of the bonded cholesterol material allows this stationary phase to be used for both reversed-phase and aqueous normal-phase separations. Interesting high selectivity is reported for the structural isomers of some antibiotics. The cholesterol bonded material does not display "phase collapse" in high aqueous content mobile phases. Variable temperature studies demonstrate that substantial structural changes of the bonded moiety occur that might be used to control selectivity. Finally, separation of some enantiomers of compounds with a variety of chemical structures is reported under reversed-phase conditions indicating that the cholesterol material may be chiral stationary phase with a broad range of applicability.

Anti-Bacterial Agents↗
PubMed2002

Modified aluminas as chromatographic supports for high-performance liquid chromatography.

This review begins by describing the relevant properties of alumina as a support material for chemically bonded stationary phases in HPLC. The most common chemical modification processes are summarized as well as the advantages and disadvantages of each method. In order to more fully understand the chemically modified alumina surface, some spectroscopic approaches are outlined for characterization of the bonded phases. Finally, a number of successful applications are described for a variety of chemically modified aluminas in order to illustrate their potential usefulness and to compare their chromatographic behavior to the more conventional silica-based materials.

Aluminum Oxide↗
PubMed2002

Synthesis and characterization of endcapped C18 stationary phases using a silica hydride intermediate.

The effect of endcapping on an octdecyl bonded phase synthesized by the silanization/hydrosilation method is investigated. The endcapping reagent is a 1:1 molar ratio of trimethylchlorosilane (TMCS) and hexamethyldisilizane (HMDS). Two approaches for endcapping are possible for this synthetic method that produces a silica hydride intermediate: bonding of TMCS-HMDS after silanization (on the hydride intermediate) or after hydrosilation (on the C18 product stationary phase). The use of TMCS-HMDS is designed to eliminate the few remaining silanols on the silica hydride intermediate. The endcapping process is characterized spectroscopically by diffuse reflectance infrared Fourier transform (DRIFT), 29Si cross polarization magic angle spinning nuclear magnetic resonance spectroscopy (CP-MAS-NMR) and 13-C-CP-MAS-NMR. The octadecyl bonded phases are characterized chromatographically by measuring the capacity factors of several hydrophobic and basic test solutes as well as the separation factors among various solute pairs. Finally, long-term stability tests are done on both products at high and low pH.

Hydrogen↗