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  • Analytical Chemistry and Spectroscopy  (16)
  • phase separation  (13)
  • 11
    Electronic Resource
    Electronic Resource
    Laser desorption time-of-flight mass spectrometric analysis of transferrin precipitated with antiserum: A unique simple method to identify molecular weight variants (1994)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 23 (1994), S. 230-233 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Serum transferrin precipitated with anti-transferrin serum was unalysed by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOFMS). The transferrin-antibody complex in the immuno-precipitates was separated into transferrin and IgG in an acidic pH, which is the usual condition of loading on MALDI-TOFMS. Ions of IgG and other minor components were not superimposed on the transferrin ions. Transferrin isoforms with different carbohydrate contents could be identified by this simple method easier than by affinity chromatography requiring the time-consuming preparation of an insolubilized specific antibody. The transferrin isoform with a molecular weight of ∼ 2.2 kDa smaller than normal transferrin, which is contained in the serum from patients with carbohydrate-deficient glycoprotein (CDG) syndrome, was identified by this method. In addition to the M1+ ion detected using sinapinic acid as a matrix, the M2+ and M3+ ions of transferrin were clearly detected using α-cyano-4-hydroxycinnamic acid as matrix and the molecular weight heterogeneity was identified more clearly in multivalent ions than that in the M1+ ion. The MALDI-TOF analysis of immunoprecipitates may serve as a simple and sensitive method to identify the molecular weight heterogeneity of various biological materials.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200230408
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  • 12
    Electronic Resource
    Electronic Resource
    Assignment of the ions in the electrospray ionization mass spectra of the tryptic digest of the non-derivatized globin, covering the whole sequence of α- and β-chains: A rapid diagnosis for haemoglobinopathy (1995)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 30 (1995), S. 1663-1670 
    Details
    ISSN: 1076-5174
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: For the rapid and simple identification of haemoglobin variants, tryptic peptides prepared by digestion of the mixture of normal and variant subunits were analysed by electrospray ionization mass spectrometry (ESI-MS). The globin was not reduced and alkylated. In a single spectrum from the ESI analysis of tryptic digests from normal adult globin, nearly 90 significant peaks were observed. Many of these peaks had the right mass and yielded tandem mass spectra of sufficient quality to define the sequence. Some ion peaks were assigned mainly by mass values with additional indirect evidence. A series of multiply charged ions were observed and these ions were valuable for making the assignments. Ion peaks which were assigned with some degree of certainty covered whole sequence from α-and β-subunits. In addition to the normal ion peaks, variant ion peaks were observed in the analysis of tryptic peptides of the non-derivatized globin mixture from Hb SC double heterozygote and from Hb MBoston heterozygote. This approach will offer routine methods in clinical laboratories.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jms.1190301205
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  • 13
    Electronic Resource
    Electronic Resource
    Pore Structure Control of Silica Gels Based on Phase Separation (1997)
    Springer
    Journal of porous materials 4 (1997), S. 67-112 
    Details
    ISSN: 1573-4854
    Keywords: pore structure control ; silica gels ; phase separation ; spinodal decomposition ; chromatography ; sol-gel
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract In the alkoxy-derived sol-gel system, various macroporous morphologies can be obtained by inducing the phase separation parallel to the sol-gel transition. This principle of macroporous morphology control can be best applied to pure silica and silica-based multicomponent oxide systems. The earlier the phase separation takes place than the sol-gel transition, the larger the characteristic sizes of pores and gel skeletons become. The time resolved light scattering measurements revealed that the morphology formation process exhibits the features of spinodal decomposition and that the final gel morphology is determined by the competitive kinetics between the domain coarsening and the structure freezing by sol-gel transition. The mesopore structure of such macroporous gel skeletons could be easily tailored by the solvent exchange procedures. Silica gels with controlled macropores and mesopores were successfully applied as a material for the continuous rod type column for high performance liquid chromatography.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009627216939
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  • 14
    Electronic Resource
    Electronic Resource
    Polymerization-induced phase separation in silica sol-gel systems containing formamide (1993)
    Springer
    Journal of sol gel science and technology 1 (1993), S. 35-46 
    Details
    ISSN: 1573-4846
    Keywords: Flory-Huggins' theory ; phase separation ; spinodal decomposition ; sol-gel method ; porous silica gel
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Silica gels with well-defined pores both in micrometer and nanometer ranges were obtained by acid-catalyzed hydrolysis and polymerization of tetramethoxysilane in the presence of formamide. The micrometer-range structures of these gels are studied in terms of the phase diagram of the quasi two-component system, namely solvent-rich and silica-rich end compositions. The resulting interconnected structures and aggregates of particles are related to the occurrence of spinodal phase separation. The composition region that gave interconnected structures for the present system was much more limited and their characteristic sizes were much smaller than those for the previously reported systems containing an organic polymer. These results could be explained qualitatively by the effect of the degree of polymerization on the Flory-Huggins' type free energy change of mixing.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00486427
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  • 15
    Electronic Resource
    Electronic Resource
    Structure Design of Double-Pore Silica and Its Application to HPLC (1998)
    Springer
    Journal of sol gel science and technology 13 (1998), S. 163-169 
    Details
    ISSN: 1573-4846
    Keywords: silica gels ; phase separation ; pore size distribution ; liquid chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Utilizing the concurrence of polymerization-induced phase separation and sol-gel transition in the hydrolytic polycondensation of alkoxysilanes, a well-defined macroporous structure is formed in a monolithic wet gel. By exchanging the fluid phase of the wet gel with an appropriate external solution, the nanometer-range structure of the wet gel can be reorganized into structures with larger median pore size essentially without affecting the macroporous framework. The double-pore structure thus prepared is characterized by open pores distributed in discrete size ranges of micrometers and nanometers. A new type of chromatographic column (silica rod) has been developed using monolithic double-pore silica instead of packed spherical gel particles. Typical silica rod columns had significantly reduced pressure drops and improved analytical efficiencies which do not deteriorate even at higher sample flow rates, both arising from a greater macropore volume than particle packed columns.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1008644514849
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  • 16
    Electronic Resource
    Electronic Resource
    Formation of Hierarchical Pore Structure in Silica Gel (2000)
    Springer
    Journal of sol gel science and technology 17 (2000), S. 191-210 
    Details
    ISSN: 1573-4846
    Keywords: silica ; phase separation ; pore structure ; mesopores ; chromatography columns
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract By inducing a phase separation parallel to the sol-gel transition of alkoxy-derived silicate systems, gels with well-defined macroporous structure can be prepared. Depending on the post-gelation treatment such as aging and solvent exchange, the final pore structure in the nanometer range of dried and heat-treated gels exhibits a considerable variation. With an aim of completely controlling the hierarchical pore structure in the discrete size ranges of nanometers and micrometers, systematic experimental studies have been performed. The macroporous nature of the wet gels allows an efficient solvent exchange process compared with conventional gels only with mesopores. In addition, the surface chemistry of the wet gel skeleton affects the mesopore formation process by the solvent exchange to a great extent. The median size of mesopores larger than 5 nm can be controlled by adjusting the basic solvent exchange conditions such as pH value, temperature and bath ratio for any kind of macroporous silica gel. On the other hand, the control of pore volume independent of the mesopore size is possible only in the system incorporated with the micelle-forming surfactant. Some examples of the effects of controlled mesopores on the analytical performance of monolithic-type chromatographic columns are also presented.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1008707804908
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  • 17
    Electronic Resource
    Electronic Resource
    Porous Gels Made by Phase Separation: Recent Progress and Future Directions (2000)
    Springer
    Journal of sol gel science and technology 19 (2000), S. 65-70 
    Details
    ISSN: 1573-4846
    Keywords: porous material ; phase separation ; microporous crystals ; chromatography
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Recent progress in the sol-gel science concerning the porous gels made by phase separation has been reviewed. Based on the principle and technique explored for monoliths, the material shape has been extended to a macroporous thick film and a macroporous gel in a confined space such as capillary, both of which are expected to find useful applications in the chromatography. The modifiable size range of the additional porosity within the micrometer-sized gel skeleton has been broadened from micropores by zeolite, mesopores by surfactant templates to macropores by intensive hydrothermal treatments. A detailed investigation of 3D interfacial structure in real space has been performed using the laser scanning confocal microscope, which enabled quantitative comparison of the structure with those of other phase-separating systems.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1008710104904
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  • 18
    Electronic Resource
    Electronic Resource
    Designing Double Pore Structure in Alkoxy-Derived Silica Incorporated with Nonionic Surfactant (1998)
    Springer
    Journal of porous materials 5 (1998), S. 103-110 
    Details
    ISSN: 1573-4854
    Keywords: silica ; sol-gel ; phase separation ; solvent exchange ; surfactant
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The principle of designing double-pore structure in alkoxy-derived silica is described with the experimental system containing polyoxyethylene nonylphenylether. The formation of macropores is consistently explained in terms of the concurrence of a phase separation and a sol-gel transition in the polymerizing silica-surfactant-solvent system. The composition-morphology relationship exhibited a substantial variation depending on the length of oxyethylene units in the surfactant molecule. The mesopore volume obtained after basic solvent exchange and a heat-treatment suggested that the surfactant with shorter oxyethylene chain tends to be incorporated more in the gel phase to give higher mesopore volume. The small-angle X-ray scattering measurement of the gelling and aging system supported this hypothesis indicating micelle formation in the system containing a surfactant with shorter oxyethylene chain.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1023/A:1009633102016
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  • 19
    Electronic Resource
    Electronic Resource
    Philanthotoxins. A mass spectrometric investigation (1989)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 3 (1989), S. 295-297 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A method employing liquid secondary-ion mass spectrometry (SIMS) in conjunction with metastable-ion measurements (linked scanning at constant B/E) to obtain sequence-specific information for three synthetic polyamine isomers was developed. The normal liquid SIMS spectra gave molecular weight information, but important sequence ions were of low intensity or obscured by the background. The metastable-ion spectra contained important fragment ions in particular due to cleavage along the polyamine chain. One of the three synthetic isomers was identical with a toxin present in the venom of the digger wasp. In conjunction with nuclear magnetic resonance spectroscopic studies, this should be a powerful method for the structural characterization of other closely related toxins present in the venom of this wasp.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290030906
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  • 20
    Electronic Resource
    Electronic Resource
    Chromatographic Properties of Miniaturized Silica Rod Columns (1998)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 477-479 
    Details
    ISSN: 0935-6304
    Keywords: Silica rod column ; micro-HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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