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  • Analytical Chemistry and Spectroscopy  (5)
  • Cyclodextrin polymer  (2)
  • Column-coupling system  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 18 (1995), S. 348-352 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Enantiomers ; Cyclodextrin polymer ; Organic modifiers ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Enantiomeric separation of some basic compounds, namely selegiline, amphetamine, and clenbuterol, was studied by capillary electrophoresis using an uncharged β-cyclodextrin polymer added to the background electrolyte at pH 2.5. Both complexation and resolution were influenced by the concentration of the chiral polymer confirming our previous results obtained in our earlier work for a wide number of pharmaceutical compounds. In this further study, we examined the influence of different organic additives to the background electrolyte on the enantioselectivity of the chiral selector, also using an extended number of analytes. In most cases, the use of an organic additive resulted in a decrease of resolution. However opposite to that, in some cases, e.g. ephedrine, the organic solvent proved to be essential to achieve enantiomeric resolution. Furthermore the influence of the capillary temperature on the resolution of the analytes was evaluated. Increase of temperature had a deleterious effect on the resolution of the enantiomers. For ephedrine, however, relatively high temperature (50 °C) proved to be advantageous, for the resolution of the optical isomers.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1040-7685
    Keywords: phytate ; capillary zone electrophoresis ; indirect UV detection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A rapid and simple analytical method was developed to determine phytate anion in soybeans. The analysis was performed by capillary zone electrophoresis with indirect UV photometric detection. The determination of phytate was carried out with a background electrolyte in which benzoate was the absorbing ion at 254 nm.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 19 (1996), S. 322-326 
    ISSN: 0935-6304
    Keywords: Capillary electrophoresis ; Enantiomer separation ; Drugs ; Loxiglumide ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Vancomycin has been used as chiral selector for the enantiomers separation of D, L-loxiglumide, a new drug proposed for the treatment of gastrointestinal pathology. The chiral selector, dissolved at very low concentration in the running buffer, filled only part of the capillary (polyacrylamide coated) and allowed chiral resolution in less than 12 min using a 50 mM phosphate buffer at pH 6. The partial separation technique allowed to obtain a detection limit of 0.5 μg/ml for each enantiomer avoiding the drop in sensitivity due to the strong UV absorption of vancomycin when present in the detector path. The effects of vancomycin concentration and buffer pH on enantiomers resolution have been studied in order to find the optimum experimental conditions for the chiral purity control of drug. The optimized method, using the internal standard, showed good reproducibility for both migration times and normalized peak area ratio and for linearity. Under the studied operating conditions it was possible to detect 0.2 % (w/w) of L-loxiglumide as a chiral impurity. Analysis of pharmaceutical preparations of D-loxiglumide did not reveal the presence of the impurity (L-isomer).
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 531-538 
    ISSN: 0935-6304
    Keywords: Capillary isotachophoresis ; capillary electrophoresis ; column-coupling electrophoresis ; enantiomers ; chiral ; amino acids ; tryptophan ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---The ability of capillary zone electrophoresis (CZE) coupled on-line with capillary isotachophoresis (ITP) sample pretreatment in the column-coupling capillary electrophoresis equipment to separate trace enantiomers present in samples of complex ionic matrices and enantiomers present in their mixtures at significantly differing concentrations has been studied. Enantiomers of 2,4-dinitrophenyl labeled norleucine (DNP-Nleu) and tryptophan enantiomers were employed as model analytes in this work while urine and mixtures of tryptophan enantiomers of differing concentrations served as model samples. Experiments performed with urine samples spiked with the DNP-Nleu racemate at sub-μmol/L concentrations demonstrated excellent sample pretreatment capabilities of ITP (concentration of the analytes, in-column and post-column sample clean up) when coupled on-line with chiral CZE separations. In the CZE separations of enantiomers present in the samples at trace concentrations the sample pretreatment could be performed in both achiral and chiral ITP electrolyte systems. The use of a chiral electrolyte system was found to be essential in the ITP pretreatment of the samples containing the enantiomers at very differing concentrations. For example, a 2×10-7 mol/L concentration of L-tryptophan could be detected in the CZE separation stage of the ITP-CZE combination in samples containing about a 104 excess of D-tryptophan only when the ITP pretreatment was carried out in the electrolyte system providing the resolution of enantiomers (α-cyclodextrin served for this purpose in the present work). A post-column ITP sample clean up was found effective in enhancing the destacking rate of the trace enantiomer in the CZE stage when the migration configuration of the enantiomers was less favorable (the trace constituent migrating behind the major enantiomer).
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 315-321 
    ISSN: 0935-6304
    Keywords: Glycopeptide antibiotics ; chiral selectors ; Teicoplanin ; enantioseparations ; CZE ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: ---Baseline separation of the enantiomers of a number of negatively charged amino and mandelic acid derivatives was achieved in less than 10 min by capillary electrophoresis in a polyacrylamide coated capillary, using the “partial filling method” (PFM) with submillimolar concentration of Teicoplanin (TE) as the chiral selector. The influence of the charge and concentration of TE, electrolyte solution composition and pH, on the enantioresolution was examined. Further proofs were brought to corroborate the hypothesis that the enantiorecognition takes place at the D-Ala-D-Ala binding site, whose blockade is responsible for the antibacterial activity of glycopeptide antibiotics. While the dependence of the chiral recognition capabilities of TE on electrolyte solution composition and pH could limit its applicability, improved sensitivity, reduction of TE wall adsorption, resulting in a good efficiency, and high cost reduction, due to the very small amount of chiral selector required, were shown as advantages of the PFM adopted in this study.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
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  • 6
    ISSN: 0173-0835
    Keywords: Capillary zone electrophoresis ; Chiral separations ; Column-coupling system ; α-Hydroxycarboxylic acids ; Sensitivity of optical detection ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: A new approach is described for highly sensitive chiral analyses by capillary zone electrophoresis, based on using an on-line combination of two capillaries filled with either chiral selective or achiral background electrolytes (BGE). Thus, the BGEs are selected in such a way that the first capillary provides optimum chiral selectivity and the second one optimum detection sensitivity. Direct chiral separations of enantiomers of mandelic, m-methoxymandelic, 3-phenyllactic and 3-indolelactic acids served as a model example for testing the approach proposed. The analyses were performed in a BGE containing acetate as a coion and L-OH-proline or aspartame as a chiral selector. For high sensitive analyses, an arrangement containing on-line combined chiral and achiral media were tested in one or two capillaries coupled via a bifurcation block. A detection limit as low as 10-18 moles was reached in the column-coupling system when the direct chiral separation was performed in the first capillary, filled with 20 mM acetate buffer, pH 4.4, containing 8 mM Cu (II) and 16 mM aspartame (L-aspartyl-L-phenylalanine methylester) and separated enantiomers were detected in the second capillary, filled with 20 mM acetate buffer, pH 3.1. The principle described is of general use in cases where the separation and detection of analytes in question require mutually different BGEs to reach the optimum selectivity and sensitivity, respectively.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 0173-0835
    Keywords: Enantiomers ; Capillary electrophoresis ; Cyclodextrin polymer ; α-Hydroxy acids ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Uncharged β-cyclodextrin polymer was used as chiral selector for the enantiomeric separation of some α-hydroxy acids by capillary electrophoresis. Complexation and enantiomeric resolution of mandelic acid, m-hydroxy and p-hydroxymandelic acid, 3,4-dihydroxymandelic acid, as well as 2- and 3-phenyllactic acid were studied, changing the concentration of the β-cyclodextrin polymer added to the background electrolyte at different pH in the range of 4.5-7. Furthermore, the effects of the concentration of the background electrolyte, column temperature, and applied voltage on chiral resolution were also examined. The best enantiomeric separations were obtained using a background electrolyte at pH 6 containing 100 mg/mL of β-cyclodextrin polymer.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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