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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 49 (1999), S. 379-384 
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; Nucleotides ; Cadmium complexation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The CE separation of twelve nucleotides (5′-mono-, di-, triphosphates of adenosine, guanosine, cytidine and uridine) was improved by adding cadmium ion to the ammonium citrate/citric acid buffer (pH 5, ionic strength 100 mM). Cadmium ion acts as a complexing agent for some nucleotides (ATP, CTP, GTP, UTP, GDP). In order to accelerate the separation, the electroosmotic flow was reversed by flushing the fused-silica capillary with 0.2 % aqueous solution of the polycationic surfactant hexadimethrine bromide. A good separation of the twelve nucleotides studied was then achieved on a dynamically coated capillary in less than 5 min by using an ammonium citrate/citric acid buffer (pH 5, ionic strength 100 mM) to which 2 mM cadmium ion has been added. High peak efficiencies were obtained (210 000 theoretical plates) and the resolution between two adjacent peaks was always greater than 1.5.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Stationary phase characterization ; Silica packing materials ; Cyclodextrins ; Partially methylated β-cyclodextrins
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The chromatographic properties of five columns packed with phenyl-bonded phases were characterized by an approach based on Tanaka's method for column to column comparisons in order to develop an LC analysis of partially methylated β-cyclodextrins. The retention behaviour of β-cyclodextrin, heptakis(2,6-di-O-methyl)-β-cyclodextrin and heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin was examined in order to evaluate the different interactions between phenyl stationary phase and this family of compound. Chromatograms show that the residual silanol activity of the packing materials plays a beneficial role in the partially methylated β-cyclodextrins separation process. It is concluded that knowledge of the interactions involved allows one to make a reasoned choice of the stationary phase in order to obtain the best possible analysis of three different commercial samples of partially methylated β-cyclodextrins.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 48 (1998), S. 739-744 
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; Nucleotides ; Inorganic cations ; Complexation with Mg and Ca
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The complexation equilibrium between nucleotides (ATP, ADP) and inorganic cations (Mg2+, Ca2+) has been studied by capillary electrophoresis. The equilibrium constant and the stoichiometry of nucleotide-inorganic cation complexes can be deduced from the dependence of the electrophoretic mobility of each nucleotide on the negative logarithm of the inorganic cation concentration. The experimental values of complexation constants determined by CE compare favorably with those in the literature. As expected, Mg2+ forms more stable complexes with ATP (logK=2.30 and 4.10 at pH 5 and 8, respectively) than with ADP (logK=1.92 and 3.15 at pH 5 and 8, respectively). In the pH range 4–8, the stoichiometry of ADP-Mg2+ and ADP-Ca2+ complexes is always 1∶1 whereas that of the complexes between these cations and ATP depends on pH-hence ATP-Mg2+ and ATP-Ca2+ complexes have 1∶1 stoichiometry at pH 5 and 1∶2 at pH 8.
    Type of Medium: Electronic Resource
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  • 4
    ISSN: 1612-1112
    Keywords: Capillary electrophoresis ; pK A determination ; Indirect UV detection ; Alkyl-alkyl phosphonic acids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Capillary electrophoresis (CE) has proved to be a fast and convenient method for the determination of the dissociation constants of non-UV absorbing solutes in the acidic pK A range (2.0–2.5). The electroosmotic flow was reversed by washing the capillary with 0.2% polybren aqueous solution. A series of background electrolytes was prepared with phenylphosphonic acid (pK A=1.29) and β-alanine (pK A=3.55) with the same ionic strength and a high buffer capacity in order to improve the repeatability (0.1–0.2 %) of the electrophoretic mobility and to determine the values of pK A accurately. This procedure was applied to the determination of the dissociation constants of several alkyl-alkylphosphonic acids whose pK A values have not yet been published in the literature. In this work, their dissociation constants have been found to vary between 1.91 and 2.34 for alkyl-methylphosphonic acids and between 2.10 and 2.38 for alkyl-ethylphosphonic acids.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' Zeitschrift für analytische Chemie 351 (1995), S. 246-250 
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Using two commercial, amino bonded, silica gel columns, binary eluents (methanol/water, acetonitrile/methanol) and ternary eluents (acetonitrile/methanol/water) are evaluated for their ability to separate oligosaccharides in comparison with classical acetonitrile/water eluents. Chromatographic data on glucose, maltose, raffinose, stachyose and maltodextrin are reported. Mobile phases consisting of acetonitrile/water or acetonitrile/methanol/water produce the best separations. Phase hydrolysis is evaluated using an evaporative light scattering detector. The reduction of the water content in the eluent stabilizes the aminocolumns and the life time of the amino columns should be improved with the ternary eluent. Moreover, a better detection limit can be obtained. Capabilties to run gradient elution without baseline drift are clearly demonstrated.
    Type of Medium: Electronic Resource
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 21 (1998), S. 554-560 
    ISSN: 0935-6304
    Keywords: LC stationary phases ; octadecyl and octylsilica characterization ; cyclodextrins ; partially methylated cyclodextrins ; heptakis(2,6-di-O-methyl)-β-CD ; evaporative light scattering detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---In order to establish guidelines to help the analyst in the choice of the most suitable octadecyl or octyl bonded phase for the LC analysis of a given partially methylated β-CD sample, analyses of four commercially available dimethyl-β-cyclodextrins (DM-β-CDs) have been carried out on nine octyl (C8) or octadecyl (C18) silica bonded or polymeric bonded phases which differ significantly in their hydrophilic and hydrophobic properties. Chromatograms show that the nature of the packing materials has considerable influence on the resolution of complex mixtures composed of closely related compounds such as partially methylated β-CDs. Among various kinds of C8 and C18 bonded phases, silica based and monomeric phases which present both reinforced hydrophobic and polar interactions showed the best performance. Whatever the complexity of the commercial DM-β-CD, the richest chromatographic fingerprints, which best depict the complexity of the mixture, are obtained with Nucleosil 50-5-C8 column. For the simplest mixtures, Nucleosil 50-5-C8 column with acetonitrile-water (34:66) as mobile phase is the most suitable chromatographic system and leads to the best resolution between heptakis (2,6-di-O-methyl)-β-CD and hexakis (2,6-di-O-methyl)-mono(2,3,6-tri-O-methyl)-β-CD (14 OCH3 and 15 OCH3). This chromatographic system might enable an LC-MS coupling for direct identification of the different components in the mixture as well as control of batch to batch variations.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 5-16 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Inorganic anions ; Decamethonium hydroxide ; Potassium dichromate ; Indirect UV detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The separation of the principal inorganic anions (bromide, carbonate, chlorate, chloride, fluoride, nitrate, nitrite, sulfate, phosphate) has been achieved using a capillary electrophoresis system with indirect UV detection at 260 nm. Several types of cationic surfactants (quaternary ammonium, phosphonium or methonium) were tested as electroosmotic flow modifiers and added to a chromatebased buffer prepared from potassium dichromate. The influence of many physicochemical parameters such as nature and concentration of cationic surfactant, buffer pH, dichromate concentration buffer, voltage and temperature upon the migration time of an analyte anion, peak efficiency, asymmetry factor, and finally resolution has been investigated. A linear relationship between the corrected area and the anion concentration in the 2.5-50 ppm range was obtained, thus allowing the quantitative analysis of anions in mineral water. Finally, by increasing the hydrodynamic injection time, the separation of inorganic anions at a low concentration level of 50 ng/ml was achieved without any loss of resolution.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
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