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  • Column liquid chromatography  (17)
  • Gas chromatography  (8)
  • Solid-phase extraction  (5)
  • Aqueous samples  (2)
  • Electrodialytic sample treatment  (2)
  • On-line preconcentration  (2)
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  • 1
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Urea herbicides ; Catalytic hydrolysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A method is described for the rapid catalytic hydrolysis of phenylurea herbicides on silica gel at elevated temperatures. After derivatisation of the anilines produced with heptafluorobutyric acid anhydride final analysis is done on a gas chromatograph equipped with an electroncapture detector. Detection limits are in the 1–5 picogram range. The method has successfully been applied to residue analysis of water samples at the 1 ppb level. The determination of free anilines present in water samples and the potential of various techniques to be used to discriminate between free anilines and parent herbicides are also discussed.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Zone-electrophoretic sample treatment ; Basic and acidic compounds ; Biological samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A modified valve arrangement for zone-electrophoretic sample treatment (ZEST)-which is coupled on-line with column liquid chromatography — is used to pretreat biological (plasma) samples. Carry-over of plasma proteins depends on the pH of the electrophoresis buffer. The determination of propranolol, metoprolol, cromolyn and salicylic acid demonstrates that both basic and acidic analytes can be isolated from the plasma matrix with high selectivity. Analogous piperazines, with different protein binding properties, were used to study the influence of protein binding on the recovery. It is shown that high protein can cause a decreased recovery.
    Type of Medium: Electronic Resource
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  • 3
    ISSN: 1612-1112
    Keywords: Gas chromatography/liquid chromatography ; Solid-phase extraction ; Water analysis ; Drying agents ; Organic contaminants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary A small cartridge containing a drying agent is inserted between a solid phase extraction (SPE) column and a gas chromatograph (GC) to enable the introduction of water-free desorption solvent into the GC in on-line liquid chromatography (LC)-type enrichment of trace-level analytes from water samples. Some characteristics of the drying agents, such as their capacity to retain water and their re-usability after heating, have been tested. Possible interactions of the drying agent with the analytes, e.g., irreversible adsorption or catalyzed degradation, have been checked for a wide range of alkanes, alkylbenzenes chlorobenzenes, chlorophenols and phthalate esters. Using the on-line SPE-GC system with flame ionization detection (FID) and spiked samples containing different levels of the test compounds, the repeatability was shown to be satisfactory (6–17%). For 10 mL samples, the detection limits were lower than 0.1 μg/L. The on-line SPE-GC-FID system here presented can be used for the repeated analysis of water samples without exchange of the dyring cartridge. The technique is applied to the analysis of tap water.
    Type of Medium: Electronic Resource
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  • 4
    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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  • 5
    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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  • 6
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Phase-transfer catalysis ; On-line derivatization ; Phenolic steroids
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Commercially available equipment from two manufacturers served to set up an automated system for the precolumn phase-transfer-catalyzed dansylation of phenolic steroids, using ethynyl estradiol (EE) and estradiol (E) as model compounds. Using different mixing techniques, the on-line determination of EE and E in 200μl untreated urine samples was achieved at a rate of 3–8 analyses per hour. Detection limits were calculated to be 3–5 ng/ml. Calibration curves in urine were linear over two orders of magnitude with r=0.999 (n=5) for EE and r=0.999 (n=6) for E. The repeatability of the determination of EE in urine (1μg/ml) was 3.9% (RSD; n=20) and of E (1.5μl/ml) 3.8% (RDS; n=10). The use of plasma instead of urine in the on-line procedures was not possible due to rapid formation of emulsions, but E and EE were determined in 100μl plasma samples using a mild off-line mixing procedure in 10min. Detection limits were calculated to be ca 10ng/ml. A reaction detector, based on a solvent-segmented system, was developed for the on-line post-column dansylation of phenols and was coupled with a reversed-phase LC system. The highly selective system showed excellent linearity over at least two orders of magnitude with r=0.9999 (n=6) for both phenol and 2,5-dimethylphenol. The reproducibility was good with RSD values of around 2%. Detection limits for loop injections from standard solutions were calculated to be between 4 and 11ng.
    Type of Medium: Electronic Resource
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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Sample treatment ; Zone electrophoresis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The design of a new valve arrangement for zone-electrophoretic sample treatment (ZEST) coupled online with high performance liquid chromatography is described. Characteristics of this valve, such as the internal heat development as a function of the current, have been investigated. By using quinidine and desipramine as model compounds it is shown that charged compounds can be isolated from biological samples, in about 15 min, with high selectivity. The carry-over of proteins to the analytical column has been compared with the carry-over using a pre-column sample clean-up method. The detection limits of quinidine and hydroquinidine (50 ng/ml), using zone-electrophoretic sample treatment coupled with column liquid chromatography, are in the same range as with direct injections using pre-columns.
    Type of Medium: Electronic Resource
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  • 8
    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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  • 9
    ISSN: 1612-1112
    Keywords: Gas chromatography ; Supercritical fluid extraction ; GC detectors ; Purity of gases
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary The usefulness of several grades of carbon dioxide for online supercritical fluid extraction/capillary gas chromatography has been studied. If trace-level work has to be performed, no single grade can be recommended for all modes of detection studied. Good-quality carbon dioxide is available for use with flame ionization and thermionic detectors. With electron-capture detection, however, distinct problems still exist.
    Type of Medium: Electronic Resource
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  • 10
    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.
    Type of Medium: Electronic Resource
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