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  • 1
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Immunoaffinity precolomn ; Oestrogens ; Bioanalysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An automated liquid chromatographic system is described using immunoaffinity precolumns for sample pretreatment. The system consists of a column-switching unit allowing preconcentration from a large volume of sample (e.g. 15 ml of urine) onto an immunoaffinity precolumn (containing polyclonal antibodies immobilized on Sepharose). After sorption, the analytes are desorbed by a mixture of two cross-reacting solutes, followed by reconcentration on a C-18-bonded silica precolumn, and then separation on a C-18-bonded silica analytical column. Using oestrogen steroids as model compounds and UV absorbance detection, the minimum detectable concentration is ca. 200 ng/l with a repeatability of 6–8%. The total analysis time is 45 min which allows the unattended analysis of 30 samples per day. The features of the sample pretreatment method, especially of the immunoselective desorption, are evaluated and the general applicability of the system is discussed.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Liquid chromatography ; Chlorophenols in water ; Preconcentration ; Post-column photochemical dechlorination ; Electrochemical, UV and fluorescence detection ; Column switching
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A specific HPLC method has been developed for the trace analysis of lower chlorinated aromatic compounds. The method consists of an on-line preconcentration and a post-column reaction step. On-line preconcentration of mono- and dichlorophenols from aqueous samples has been performed using PRP1, a divinylbenzene-styrene copolymeric sorbent as packing material for both pre-and analytical column. Enrichment factors of over 300 were obtained compared to regular (100 μl) loop injections, even for the highly polar monochlorophenols. After reversed-phase separation, post-column photochemical dechlorination is carried out directly in the eluent stream, using a photochemical reactor. Upon dechlorination, fluorescent products are formed, which can be detected selectively. The resulting fluorescence signal shows a linear response to the quantity of solute present over 2 to 3 orders of magnitude (correlation coefficients: 0.990–0.98). For the mono- and dichlorophenols, the detection limit of the photoconversion method is in the lower nanogram range. The method is especially suitable for the analysis of complex matrices such as effluent water samples or biological fluids containing traces of the polar chloroaromatic compounds together with large amounts of other constituents, which interfere when using more general methods of detection like UV absorption. The potential of this technique for automation has been demonstrated by using a microprocessor-controlled column switching unit.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 2 (1979), S. 11-14 
    ISSN: 0935-6304
    Keywords: Liquid chromatography ; Fluorescence ; Ion-pair extraction ; Amines ; Post-column reaction ; Auto-analyser ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A detection system is described which is based on fluorescent ion-pair formation between tertiary amine drugs and dimethoxyanthracene sulphonate. A dynamic micro-extraction principle is then used to isolate the ion-pairs from the excess reagent. The band broadening of this extraction detector was kept below 20% using standard auto-analyser equipment. With the enhanced selectivity and sensitivity of this approach it was possible to analyse chloropheniramine in urine at ppb concentrations using a pre-column clean-up trace enrichment step.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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