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  • Capillary zone electrophoresis  (1)
  • Cyclodextrin modified - micellar electrokinetic chromatography  (1)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Electrophoresis 19 (1998), S. 2883-2889 
    ISSN: 0173-0835
    Keywords: Tramadol ; Enantiomers ; Cyclodextrins ; Capillary zone electrophoresis ; Validation ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: Capillary zone electrophoresis was successfully applied to the enantiomeric resolution of racemic tramadol. Both uncoated and polyacrylamide-coated capillaries were tested for method optimization using either negatively charged or native cyclodextrins (CD) added to the background electrolyte (BGE). The resolution was strongly influenced by the CD type and concentration as well as by the pH and the concentration of the BGE. Among the CDs tested, carboxymethylated-β-cyclodextrin allowed the baseline separation of tramadol enantiomers. After the method was optimized, it was validated in a coated capillary for enantiomeric analysis of tramadol enantiomers in pharmaceutical formulation, including specificity and elution order, linearity, accuracy and precision, determination of limit of detection (LOD) and quantification (LOQ), enantiomeric purity linearity, freedom from interference, and stability of sample solutions. Precision at the target concentration was less than 2%, with an accuracy higher than 99%. Furthermore, the method was able to detect 0.3% and to quantify 1% of the minor enantiomer in the presence of the major one at the target value.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0173-0835
    Keywords: Cyclodextrin modified - micellar electrokinetic chromatography ; Chiral separation ; Chrysene metabolism ; Chemistry ; Biochemistry and Biotechnology
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Biology , Chemistry and Pharmacology
    Notes: A γ-cyclodextrin (γ-CD) modified electrokinetic micellar capillary chromatography (MEKC) method was used for the enantiomer separation of a racemic trans-1,2-dihydro-1,2-dihydroxy-chrysene (chry-trans-1,2-diOH) mixture. The chiral resolution was strongly influenced by several important parameters: surfactant concentration and addition of organic modifier to the background electrolyte (BGE). An optimized electrophoretic system was used, consisting of the following conditions: 25 mM phosphate buffer, pH 7.8, 50 mM sodium dodecyl sulfate, 20 mM γ-CD, 7.4% V/V 2-propanol as BGE; the applied voltage, 18 kV, corresponded to 37 μA at a constant temperature of 25°C. This electrophoretic method was applied for monitoring the chry-trans-1,2-diOH enantiomer formation in a real sample, obtained from in vitro metabolic activation of chrysene by phenobarbital-ß-naphthoflavone-induced rat microsomes. The (+) and (-) enantiomers were identified by the racemate and the single enantiomer standard addition method and by spectra comparison with the synthetic compound. Under the experimental conditions used for chrysene activation, the (+) optical isomer was the prevailing form. The CD-MEKC system showed high reproducibility and selectivity, allowing a fast and interference-free analysis even of the in vitro metabolic sample extract, without any pretreatment.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
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