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  • 1
    Electronic Resource
    Electronic Resource
    Amsterdam : Elsevier
    Analytica Chimica Acta 266 (1992), S. 233-241 
    ISSN: 0003-2670
    Keywords: Chemiluminescence ; Copper ; Metal ions ; Peroxyoxalate chemiluminescence
    Source: Elsevier Journal Backfiles on ScienceDirect 1907 - 2002
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Membrane-extraction disks ; On-line trace enrichment ; Polar pollutants ; Surface water
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An on-line trace-enrichment system, using a bifunctional membrane extraction-disk cartridge, has been combined with a column liquid chromatography separation for the simultaneous determination of basic, neutral and acidic pollutants in surface water. The enrichment device consisted of a specially constructed holder containing both C-18 and cation-exchange disks. The holder can contain up to 25 disks of 0.5 mm thickness and 4.6 mm diameter. Before trace enrichment of 20 ml of surface water (pH 3.0), calcium ions were removed from the sample by means of an oxalic acid precipitation. Desorption of the cartridge was at elevated temperature using reversed-phase gradient elution; detection was performed with a diode-array UV absorbance detector. The detection limits for the test compounds in surface water are typically 0.5–2 μg/l; the calibration graphs are linear from the lower limit of determination up to 50 μg/l.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Two-dimensional separation ; D- and L-amino acids ; Enantioseperation
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A two-dimensional, column liquid chromatographic system is used for the determination of the D- and L-enantiomers of amino acids in biological samples. Separation of the amino acids is first on ion-exchange column by gradient elution with a sodium citratesodium chloride buffer. Enantioseparation is by subsequent injection of 3 μl heart-cuts of the individual amino acids onto a second column with a chiral crown ether stationary phase. Finally, fluorescence detection is after post-column labelling of the amino acids using ano-phthalaldehyde-2-mercaptoethanol reagent solution. The high separation power and selectivity of the system allow processing of complex samples with hardly any additional treatment and the determination of small quantities of D-amino acids in the presence of excess L-form. Applicability of the system is illustrated by the determination of D- and L-aspartate, serine, glutamate and alanine in various complex biological samples, such as protein hydrolysates, urine and biotechnological and food samples. Data are given on detectability, repeatability and linearity.
    Type of Medium: Electronic Resource
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  • 4
    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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  • 5
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; On-line preconcentration ; Polar pollutants ; Water (tap and surface)
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An isocratic column liquid chromatographic system with UV absorbance detection at 230 nm has been developed for the rapid trace-level determination of a large number of polar pollutants in water. The systems contains two precolumns, in series, which are packed with a styrenedivinylbenzene (PLRP-S) polymer. The second precolumn is also loaded with sodium dodecylsulphate before use. Each precolumn is combined with a PLRP-S analytical column, and aqueous acetonitrile mixtures (pH 3) are used for the separation of neutral as well as acidic and basic pollutants. With 10-ml water samples the detection limits for all analytes, in tap water, are in the low to sub μg/l range. Relevant analytical data are reported and the advantage of using a dodecylsulphate-loaded precolumn over a cation-exchange precolumn is discussed.
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  • 6
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Polar pollutants in water ; On-line trace enrichment ; Humic substances
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A practical liquid chromatographic early-warning system for polar pollutants in water ought to have detection limits at a level below a microgram per litre. Using ultraviolet absorbance detection this normally necessitates trace enrichment of the samples. In this study ten different sorbents have been tested with respect to their enrichment capacity. The hydrophobic polymeric PLRP-S material, in combination with a C-18 modified analytical column, proved to be the best choice. The influence of humic substances, present in surface water, was also studied. Lowering of the sample pH, resulted in a significant increase in the interferences due to the humic substances.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Precolumn derivatization ; Dansylhydrazine ; Fluorescence detection ; Tacrolimus (FK 506) in blood
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A sensitive and selective liquid chromatographic method, using precolumn derivatization with dansylhydrazine followed by fluorescence detection, has been developed for the determination of tacrolimus (FK 506) in whole blood. After haemolysis, whole blood samples are extracted with diethyl ether and derivatized. After on-line removal of excess dansylhydrazine on a C18 precolumn, the derivative is loaded on to a C18 clean-up column, and a heart cut is subsequently transferred to a graphitized carbon column, where the final separation takes place. The method requires 1 ml of sample and has a limit of quantitation of 3 ng/ml. At the 15 ng/ml level the precision isca 10%, and the response is linear from the limit of quantitation toca 200 ng/ml of FK 506 in whole blood. The capacity of the method is 50 samples/day and about 1000 1-ml samples can be analyzed without changing either clean-up or separation column. Finally, the applicability of the method for therapeutic drug monitoring is shown.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ion-pair chromatography ; Valve switching ; Fluorouracil
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Fluorouracil has been analyzed with a reversed-phase ion-pair liquid chromatographic system applying PRP-1 as the stationary phase. A valve switching technique was applied for the separation of the analyte and some other chemotherapeutic agents. The described procedure gives a rapid screening for the analyte in urine and plasma samples without interferences from late eluting solutes. Biological samples are pretreated by means of a liquid-liquid extraction resulting in a recovery of about 52% for plasma and urine with minimum detectable amounts of about 5ng/ml. The sensitivity and the selectivity of the procedure allows the monitoring of fluorouracil in body fluids and subsequent pharmaco-kinetic studies of the fluoropyrimidine.
    Type of Medium: Electronic Resource
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  • 9
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Trace enrichment ; Membrane extraction disks ; Triazine herbicides ; 2,3,4-Trichlorophenol
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Membrane extraction disks have been recently introduced for the solid-phase extraction of organic compounds from aqueous samples. The material consists of alkyl-modified silica particles enmeshed in an inert PTEE matrix. Aqueous samples containing polar pesticides and herbicides, are preconcentrated on-line from acidic solutions on membrane extraction disks containing immobilized octadecyl-modified silica and analyzed with an isocratic liquid chromatographic system using PLRP-S as the stationary phase and aqueous acetonitrile mixtures (pH 3) as the eluent. Data on the lifetime and the dimensions of the preconcentration disks, and the efficiency and the repeatability of the procedure are reported. For 10 ml samples, the detection limits of the analytes atrazine, simazine and 2,3,4-trichlorophenol in tap water are 0.1–1 ppb.
    Type of Medium: Electronic Resource
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  • 10
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Ultrafiltration ; Fermentation monitoring ; Sugars
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An automated on-line monitoring system for low-molecular-weight compounds (e.g. sugars) during fermentation processes is described. The applicability of cross-flow ultrafiltration, coupled on-line with high-performance liquid chromatography, is evaluated. Various detection modes for the determination of the test compounds lactose, glucose and fructose) in a complex fermentation broth are compared. In addition, the influence of some system parameters on the performance of several ultrafiltration modules for the removal of cellular and macromolecular broth constituents is investigated. A method for the fully automated determination of sugars during anE. coli batch culture in a brain-heart infusion medium is presented. With the present system five analyses can be performed every hour, using only 35μl of sample, without significant deterioration of the ultrafiltration process. Contamination by external micro-organisms was not observed and good correlation with an off-line method was found.
    Type of Medium: Electronic Resource
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