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  • 1
    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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  • 2
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Electrodialytic sample treatment ; Computer models ; Analyte enrichment
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Basic considerations for analyte enrichment and recovery obtainable by electrodialysis as a sample treatment method are given. Equations are derived which describe the dependence of the concentration profiles of ionic compounds on the electric field strength in a set-up with stagnant donor and acceptor solutions. It is shown that analyte recovery increases when less ion-selective membranes are used in the electrodialysis cell. Computer models are used to estimate the analyte enrichment for a flowing donor (sample) and a stagnant acceptor phase. About 10-fold enrichment can be obtained in an electrodialytic sample treatment system within 20 min under maximum current conditions. A compromise has to be found between analyte recovery and the donor (sample) flow rate.
    Type of Medium: Electronic Resource
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  • 3
    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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  • 4
    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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  • 5
    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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  • 6
    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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  • 7
    ISSN: 1612-1112
    Keywords: Column liquid chromatography ; Gas chromatography-mass spectrometry ; Water analysis ; Triazine herbicides ; Chemical ionization mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Mass spectra of 12 triazines were obtained by electron impact (EI), positive-ion chemical ionization (PCI) and negative-ion chemical ionization (NCI) using methane and isobutane as reagent gases. EI mass spectrometry is more sensitive than PCI and NCI, although the chemical ionization modes increase selectivity markedly. A pre-column packed with polymer stationary phase was employed to preconcentrate surface and drinking water samples. After desorption of the analytes with ethyl acetate, an aliquot was injected directly into the GC-MS system. Atrazine and simizine were found in these samples at 10–80 ppt levels. The limits of detection for both herbicides were below 10 ppt in drinking water.
    Type of Medium: Electronic Resource
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  • 8
    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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  • 9
    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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  • 10
    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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