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  • Electrochemical detection  (1)
  • Enantiomers  (1)
  • 1
    ISSN: 1612-1112
    Schlagwort(e): Terbutaline ; Plasma ; Automated HPLC ; Column-switching ; Electrochemical detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An automated method based on liquid chromatography has been developed for the determination of terbutaline in human plasma in the range of 5–50 pmole·ml−1. The necessary sensitivity and selectivity was obtained by using electrochemical detection and a microprocessor-controlled column switching system. A combination of three columns was used: a C8 type for pre-separation, a C18 type for trapping and, for final separation, a strongly acidic ion exchanger. The accuracy of the method was examined by comparison with a method based on gas chromatography — mass spectrometry. The overall precision was ±3.5% and ±2.2% respectively at 5 and 50 pmole·ml−1. The total absolute recovery for terbutaline and internal standard at the above concentration levels were in the range 85–106%.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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  • 2
    ISSN: 1612-1112
    Schlagwort(e): Liquid chromatography ; Coupled columns ; Cyclodextrin ; Enantiomers ; Chiral separation ; Bioanalysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary β-cyclodextrin was used in the mobile phase as chiral selector for separating the enantiomers of terbutaline, chlorthalidone and oxazepam. The effect on chiral resolution using e.g. hydrophobic, polar or cation exchanging stationary phases was investigated. Both the chiral separation factor and retention level were affected by the concentration of methanol and β-cyclodextrin. The stationary phase had no effect on the chiral separation only on the level of retention. By tuning the concentration of β-cyclodextrin and methanol in the mobile phase chiral separation could be obtained on most stationary phases. By changing the stationary phase while adjusting the mobile phase composition to maintain the chiral selectivity, improvements of the selectivity towards e.g. endogenous compounds can be obtained when separating enantiomers in complex matrixes as biological fluids. Further improvement on selectivity can be obtained if coupled columns are used. This is examplified for separation of chlorthalidone and terbutaline enantiomers in biological fluids by coupling an achiral column to another achiral column and using a mobile phase containing β-cyclodextrin on the last column.
    Materialart: Digitale Medien
    Bibliothek Standort Signatur Band/Heft/Jahr Verfügbarkeit
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