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  • 1
    ISSN: 1432-0614
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract An automated system for the monitoring of fermentations of filamentous fungi is described. The system is based on the on-line combination of ultrafiltration, for the removal of cellular and macromolecular material from the fermentation broth, and column liquid chromatography for analysis of the filtrate. The performance of one hollow-fibre and two planar ultrafiltration modules is evaluated. The maximum sampling frequency as well as prevention from clogging by mycelium is strongly dependent on the construction of the module, best results being obtained with a planar membrane and a relatively high flow rate (150 ml/min) of the broth through a single, wide-bore (3 mm) flow channel in the module. The method is used for the study of metabolic and regulatory processes of two different Aspergillus niger strains on multiple carbon sources. The selected system can be applied for at least 70 h without any negative effect on either the fermentation or the analytical system. Through an analysis frequency of once per hour detailed information regarding consumption and production of nine different compounds could be obtained.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 1432-0614
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Abstract An automated system for the monitoring of fermentations of filamentous fungi is described. The system is based on the on-line combination of ultrafiltration, for the removal of cellular and macromolecular material from the fermentation broth. and column liquid chromatography for analysis of the filtrate. The performance of one hollow-fibre and two planar ultrafiltration modules is evaluated. The maximum sampling frequency as well as prevention from clogging by mycelium is strongly dependent on the construction of the module, best results being obtained with a planar membrane and a relative high flow rate (150 ml/min) of the broth through a single, wide-bore (3 mm) flow channel in the module. The method is used for the study of metabolic and regulatory processes of two different Aspergillus niger strains on multiple carbon sources. The selected system can be applied for at least 70 h without any negative effect on either the fermentation or the analytical system. Through an analysis frequency of once per hour detailed information regarding consumption and production of nine different compounds could be obtained.
    Type of Medium: Electronic Resource
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  • 3
    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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  • 4
    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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  • 5
    ISSN: 1612-1112
    Keywords: Thermospray MS-MS ; Flow injection analysis ; Phenoxyacid herbicides ; Surface waters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Optimization of signal-to-noise ratios (S/N) by optimizing electron multiplier (EM) voltage and resolution of the first and second mass analyser in a thermospray (TSP), tandem mass spectrometer system is studied. Using flow injection analysis (FIA) of samples containing eight chlorophenoxy carboxylic acid herbicides and bentazone, and a FIA system, the signal and background (noise) intensity i.e. S/N are studied with selected reaction monitoring (SRM) at different EM voltages. An EM voltage of 2500 V improves the S/N ratios 5.5–13 fold compared to the usual 1700 V. Applying additional resolution voltages of +3 to +4 V to the first and second mass analyser decreases resolution in each mass analyser, but there is no overall loss in selectivity, while the S/N ratios further increase 3–4 fold. The selectivity of measurements was studied using 2,4,5-T ((2,4,5-trichlorophenoxy)acetic acid) and triclopyr, which differ only one mass unit in the selection of the parent and daughter ion mass in the applied SRM method. Resolution could be decreased to 36–54% valley definition, while still ensuring the selectivity. With the herbicides studied, screening of surface water samples spiked at the 1 μg l−1 level, corresponding to 25 pg component s−1 into the MS, is easily achieved under optimum conditions without analyte concentration. Some sample clean-up is recommended, however, because ionization efficiencies tend to diminish with some of the raw sample studied.
    Type of Medium: Electronic Resource
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  • 6
    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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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrodialytic sample treatment ; On-line coupling
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An electrodialytic sample treatment method coupled on-line with high-performance liquid chromatography (EDIST-HPLC) is discussed in this paper. The performance of EDIST as a function of the donor-phase (sample solution) flow rate, the voltage applied over the electrodialysis block, and the time of dialysis has been studied using the basic drug ephedrine as a model compound. Enrichment of the analyte by a factor of 10–20 was possible. The determination of human plasma spiked with ephedrine is briefly discussed.
    Type of Medium: Electronic Resource
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  • 8
    ISSN: 1612-1112
    Keywords: Coupled LC-GC-MS ; Polycyclic aromatic hydrocarbons ; Vegetable oil samples
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary An on-line combination of liquid chromatography, gas chromatography and mass spectrometry has been realized by coupling a quadrupole mass spectrometer to an LC-GC apparatus. Liquid chromatography was used for sample pretreatment of oil samples of different origin. The appropriate LC fraction, containing polycyclic aromatic hydrocarbons, was transferred to the gas chromatograph using a loop-type interface. After solvent evaporation through the solvent vapour exit and subsequent GC separation, the compounds were introduced into the mass spectrometer for detection and identification. The GC column was connected to a short piece of deactivated fused silica that protruded into the ion source. The total analytical set-up allowed the direct analysis of oil samples after dilution in n-pentane without any sample clean-up. Detection limits are about 40 pg in the full scan mode and about 1 pg with selective ion monitoring, i.e. 20 ppb and 0.5 ppb respectively.
    Type of Medium: Electronic Resource
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  • 9
    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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  • 10
    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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