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  • 1
    Electronic Resource
    Electronic Resource
    A Multidimensional Approach to Protein Characterization (1997)
    Springer
    The protein journal 16 (1997), S. 523-526 
    Details
    ISSN: 1573-4943
    Keywords: Mass spectrometry ; deuterium exchange ; two-dimensional separations ; secondary structure ; protein: ligand interaction
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract When mass spectrometry (MS) is used to study protein primary structure, it is used in a “static” mode. That is, the information is derived from a single MS or MS-MS spectrum. Information about more complex protein structure or protein interactions can also be gained via MS. If a series of mass spectra is collected as something else in the experiment is changing, we increase the “dimensionality” of the MS data. For example, measuring mass spectra as a function of time after exposure of a protein to deuterated solvents can provide information about protein structure. Likewise, by measuring mass spectra of a protein as the concentration of a binding ligand is changed, one can infer the stoichiometry of the complex. Another important, but fundamentally different way of increasing the dimensionality of mass spectral data is by coupling the mass spectrometer to a one- or two-dimensional separation technique.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1026373830301
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  • 2
    Electronic Resource
    Electronic Resource
    Capillary zone electrophoresis for the determination of electrophoretic mobilities and diffusion coefficients of proteins (1989)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 1 (1989), S. 41-45 
    Details
    ISSN: 1040-7685
    Keywords: capillary electrophoresis ; mobility ; diffusion coefficient ; proteins ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary zone electrophoresis can be used to determine mobilities and diffusion coefficients for analytes. Mobilities are determined from measurements of migration times. Correction for electroosmotic flow must be made by measuring the flow magnitude using an uncharged marker substance. Diffusion coefficients can be measured from peak widths of analyte bands. Care must be taken in these measure- ments that the analyte concentration does not overload the system and perturb the axial homogeneity of the electric field strength. Analyte also must not adsorb to the surface of the capillary. Finally, the capillary should be operated with a power dissipation that is low enough that minimal heating of the capillary occurs. Capillary zone electro- phoresis offers some advantages over other methods of determining mobilities and diffusion coefficients. These include a requirement of only small quantities of analyte at relatively low concentrations and the capability of making measurements on several substances simultaneously in mixtures.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220010110
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  • 3
    Electronic Resource
    Electronic Resource
    A comparison of tryptic digests of bovine and equine cytochrome C by comprehensive reversed-phase HPLC-CE (1990)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 2 (1990), S. 293-299 
    Details
    ISSN: 1040-7685
    Keywords: multidimensional separations ; two-dimensional separations ; CZE ; capillary electrophoresis ; peptide fingerprinting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Comprehensive two-dimensional reversed-phase HPLC-capillary electrophoresis (RP HPLC-CE) was used to compare the tryptic digest fingerprints of horse heart cytochrome C and bovine heart cytochrome C. The peptide fragments were labeled with fluorescamine and detected with a fluorescence detector. The two-dimensional separation system proved to be reproducible enough to identify some species differences in the tryptic digest fingerprints. Improvements in instrumentation and daily procedures yielding faster analysis times and better reproducibility compared to a previous system are described. Improvements in software yielding gray-scale images of the two-dimensional data are described. Identification of selected tryptic fragments was achieved.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220020607
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  • 4
    Electronic Resource
    Electronic Resource
    Microcolumns and ultramicro analysis (1989)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 1 (1989), S. 268-269 
    Details
    ISSN: 1040-7685
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220010603
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  • 5
    Electronic Resource
    Electronic Resource
    Evaluation of etched borosilicate glass capillary columns in reversed phase open tubular liquid chromatography (1991)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 3 (1991), S. 311-317 
    Details
    ISSN: 1040-7685
    Keywords: open tubular liquid chromatography ; capillary liquid chromatography ; column efficiency ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The performance of etched borosilicate capillary columns with a bonded octadecyl stationary phase has been examined. Plate heights for three test compounds in columns with inner diameters between 6.5 and 14.6 μm were measured as a function of mobile phase velocity. The reduced plate height vs. reduced velocity curves were then fit to the Golay equation using nonlinear regression analysis. It was found that in addition to longitudinal diffusion in the mobile phase, longitudinal diffusion in the stationary phase was a significant contributor to broadening at low mobile phase flow rates. At higher flow rates, resistance to mass transfer in the stagnant mobile phase in the porous glass produced by the etching procedure became measurable.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220030404
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  • 6
    Electronic Resource
    Electronic Resource
    Effects of methanol-modified mobile phase on the separation of isotopically substituted compounds by micellar electrokinetic capillary chromatography (1989)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 1 (1989), S. 125-130 
    Details
    ISSN: 1040-7685
    Keywords: micellar electrokinetic capillary chromatography ; capillary electrophoresis ; isotopic separations ; micellar separations ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Near-baseline resolution of dansylated methylamine and dansylated methyld3-amine can be achieved by micellar electrokinetic capillary chromatography (MECC) utilizing a 25-mM sodium dodecylsulfate pseudostationary phase and a mobile phase containing 4.9 M methanol. This study examines the role of methanol on this separa- tion by looking at its effects on to, tr,tm, and resolution over four methanol concentrations, 0 M, 2.5 M, 4.9 M, and 7.4 M. The 4.9 M methanol buffer proves to be the best for optimizing the resolution of these two extremely similar compounds. Because of the high organic content of the mobile phase, it is unreliable to determine tm based upon the migration time of a single species. A method for determining tm based upon a homologous series of standards is presented and examined over the four methanol concentrations. Plots of log k′ versus carbon number yield straight lines with similar slopes for each of the four buffer systems, indicating that this procedure is a good method for tm determination.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220010304
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  • 7
    Electronic Resource
    Electronic Resource
    Preparation of reversed phase open tubular liquid chromatographic columns from borosilicate glass (1991)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 3 (1991), S. 303-309 
    Details
    ISSN: 1040-7685
    Keywords: open tubular liquid chromatography ; column preparation ; capillary column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation of open tubular liquid chromatographic columns with small inner diameters (≤ 20 μm) from Pyrex 7740 borosilicate glass is described. The surface area of the inner wall of the capillary is increased by etching with a series of acidic and basic solutions. Dimethyloctadecylchlorosilane is then reacted with the column wall to create a bonded stationary phase layer. The resulting columns exhibit good retention and high efficiency. The effects of each step in the etching process are examined and the silanization reaction is optimized.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220030403
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  • 8
    Electronic Resource
    Electronic Resource
    Preparation and evaluation of an on-line preconcentrator for capillary electrophoresis (1993)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 5 (1993), S. 325-330 
    Details
    ISSN: 1040-7685
    Keywords: On-line preconcentration ; capillary zone electrophoresis ; sensitivity enhancement ; micro electric are discharge ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The preparation and performance of an on-line preconcentrator for capillary electrophoresis (CE) is described. Borosilicate glass microspheres were dry-packed into the fused silica column terminus and sintered in place with a micro electric are developed for this application. Reversed-phase LC packing material was slurry-packed onto this frit, in lengths of 1-3 mm. An additional frit of borosilicate beads behind the preconcentrator was used to fix the packed bed in place. The performance of the packed bed preconcentrator for the enhancement of UV and fluorescence detection limits was evaluated. Construction of the micro electric are device, the packing procedures, and practical applications are described.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220050405
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  • 9
    Electronic Resource
    Electronic Resource
    Efficiency of packed microcolumns compared with large-bore packed columns in size-exclusion chromatography (1990)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 2 (1990), S. 120-126 
    Details
    ISSN: 1040-7685
    Keywords: size-exclusion chromatography ; protein separations ; packed microcolumn liquid chromatography ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Columns with inner diameters of 50 and 28 μm were slurry-packed with 4-5 μm size-exclusion chromatography particles (Du Pont GF 250 Zorbax Bioseries) and compared with a commercially prepared 9.4-mm i.d. column that was packed with the same particles. The columns were compared on the basis of efficiencies, peak shapes, and van Deemter coefficients obtained for three proteins used as test analytes. The microcolumns provided more symmetrical peak shapes and lower plate heights than those provided by the commercial column if the peaks were analyzed using statistical moments. For example, hmin for bovine serum albumin was 5.6 in the commercial column and 2.1 in the microcolumn. This difference is attributed to the quality of the packing process, based on the fact that the van Deemter A term was significantly lower for the microcolumn than for the conventional column. The van Deemter data demonstrate that the A term was the major source of band broadening in the commercial column throughout the range of velocities used, and both the A and C terms were significant for the microcolumn. A 90 cm × 50 μm column was prepared and showed approximately 80% of the expected increase in efficiency.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220020307
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  • 10
    Electronic Resource
    Electronic Resource
    Design of a coaxial continuous flow fast atom bombardment probe (1988)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 2 (1988), S. 100-104 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290020510
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