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  • 1
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbohydrates ; Anomer separations ; Post-column derivatization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive post-column fluoresence method based on the reaction of reducing sugars with a fluorigenic reagent (benzamidine) under alkaline conditions and elevated temperature is described. Optimum reaction conditions suitable for the detection of fluorescent reaction products have been investigated. A porous graphitized carbon column (shandon Hypercarb) was employed as the chromatographic solid phase and elution was isocratic by an aqueous acetonitrile mixture. A special problem in sugar analysis is the tendendy of anomer formation giving doublet peaks. This tendency varies largely among the different sugars, and systematic studies on conditions that eliminate this problem were performed. Efficient and selective separations of a series of disaccharides were obtained using high temperatures and a low concentration of acetonitrile in the mobile phase. The detection limits (S/N=3) with an injection volume of 20 μL ranged from 10–60 picomoles. Linear calibration graphs were obtained in the 2–20 μM concentration range (r 2〉0.99). A relative standard deviation between 1–3% (n=6) demonstrated good precision of the developed system.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Ligand exchange chromatography ; Carbohydrates ; Alkaline pH ; Metal complexation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary At alkaline pH, carbohydrates are highly retained on a sulphonated polystyrene resin loaded with rare earth or uranyl metal ions. The complex formation is governed by the ionization of the carbohydrate moiety. pH and the type of metal ion were found to have a decisive influence on the complex formation. Binding of the metal ion to the cation exchanger and to different carbohydrates is described. The competitive complexation between solute and hydroxide to the metal ions is described as a ligand exchange reaction and a retention model is proposed. The ligand exchange column was used as precolumn in a coupled column separation system and the high selectivity is demonstrated by the separation of paracetamol glucuronide from a urine sample after filtration and direct injection.
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Chromatographia 35 (1993), S. 55-60 
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Carbohydrates ; Ion-pair separation ; Glycoconjugates ; PRP-1 and PLRP-S
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A new technique for the separation of carbohydrates as ion-pairs in strongly alkaline solution is presented. Carbohydrates are weakly acidic and partly present as anions at pH≥12 [1]. They are retained as ion-pairs on polymeric solid phases (PRP-1 and PLRP-S) with a hydrophobic quaternary ammonium counter ion present in the mobile phase. The effects of nature and concentration of mobile phase components on the retention of carbohydrates have been investigated and an ion-pair distribution model is proposed. The influence of temperature indicated no changes in retention mechanism with high counter ion concentration, but the resolution decreased with increasing temperature. Saccharides added to the mobile phase were shown to increase the retention and the selectivity.
    Type of Medium: Electronic Resource
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