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  • Column liquid chromatography  (7)
  • Surface physics, nanoscale physics, low-dimensional systems
  • 1985-1989  (7)
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Verlag/Herausgeber
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Jahr
  • 1
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 21 (1986), S. 205-213 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Chiral phases ; Optimization of separation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The preparation and properties of chiral bonded phases with amino acid groups are described. These phases were used in non-polar eluents and in aqueous systems in the presence of Cu2+ ions in the ligand-exchange mode. The optimization of chiral resolution is demonstrated for both cases. With non-polar eluents similarity between bonded groups and solutes is required. The elution could be accelerated by non-protonic moderators. Ligand-exchange separation is influenced by the copper content of the eluent and the stationary phase, the organic moderator concentration, the pH and ionic strength of the buffer and by the temperature. Structural requirements of both the bonded groups and of the solutes for chiral separation are discussed.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 2
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 25 (1988), S. 791-796 
    ISSN: 1612-1112
    Schlagwort(e): Gel permeation ; Column liquid chromatography ; Column switching ; Additives in cellulose acetate
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The capability of elution-elution multi-dimensional liquid chromatography was investigated. A “column scaling” approach was evaluated for the quantification of low-molecular-weight additives in cellulose acetate. A small-bore (1-mm i.d.) gel-permeation column was used to separate the higher-molecular-weight polymer from the lower-molecular-weight components. Once separated these additives were transferred to a C18 reversed-phase column via a switching valve. The reversed-phase system successfully separated and quantified individual additives. Analysis time for an ultraviolet inhibitor, Tinuvin®P, in cellulose acetate, including re-equilibration, was approximately 30 minutes. Both accuracy and precision were good. Precision over a three day period was about 1.5%.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 3
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Phase-transfer catalysis ; On-line derivatization ; Phenolic steroids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: 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.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 4
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 27 (1989), S. 225-227 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reverse-phase chromatography ; Elastin Hydrolysis measurement ; On-line post-column derivatization
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Excessive breakdown of elastin, a structural protein, may be related to aortic disease and emphysema. Since L-valyl-L-proline occurs in high concentrations in elastin, a rapid and sensitive method using HPLC with post-column on-line derivatization was used to measure the dipeptide from swine aortic tissue, and the amount of elastin present was determined. Elastin was extracted by alkaline hydrolysis. After neutralization and filtration, the sample was injected onto a ODS-2 gel column, and the dipeptide was eluted by a linear gradient of 0 to 10% of 1-propanol in 50 mM heptafluorobutyrate, pH 3, at a flow rate of 1 ml/min. The eluent was reacted with fluorescamine at pH 8.6, and fluorescence was detected at an excitation wavelength of 395 nm and a 455 nm cutoff emission filter.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 5
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Reversed-phase system ; On-line post-column extraction ; Electron-capture detection
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A post-column extraction module has been used for the on-line coupling of conventional-size (4.6mm i.d.) reversed-phase liquid chromatography (PPLC) and electron-capture detection (ECD). Hexane and toluene were used as extraction solvents, while methanol turned out to be preferable to dioxane and acetonitrile as modifier in the aqueous eluent. In this system the ECD behaves as a concentration-sensitive detector. The band broadening in the evaporation interface, which connects the extraction module with the ECD, dominates the total post-column band broadening; it can be reduced to 3–4 sec by directing at least 0.25–0.30 ml/min (i.e. 25–30%) of the extraction solvent to the ECD. Optimal signal-to-noise ratios were observed if 30–60% of the extraction solvent is directed to the ECD. The noise levels are 5–10 times higher than in systems using a direct coupling of normal-phase LC or narrow-bore reversed-phase liquid chromatography to the ECD. Separations of phenylurea herbicides and chlorophenols demonstrate the applicability of the RPLC-extraction module-ECD system.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 6
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Expert systems ; Optimization of operating parameters
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Given the mobile and the stationary phase and values for the physical parameters such as temperature and pH, a separation can be optimized by varying the so-calledchromatographic parameters. These include the column dimensions, particle size, operating conditions (e.g. flow rate, attenuation) and instrumentation (e.g. detector cell, time constant). Optimization of the chromatographic parameters implies finding the best possible set of values, which we define as yielding (i) sufficient separation and (ii) sufficient sensitivity in (iii) the shortest possible time. Finding the best possible conditions (the global optimum) is very difficult for chromatographers in practice. An expert system is described that allows chromatographic optimization to be performed for isocratic separations. An initial chromatogram is required to consult the system. In return, the system provides a complete set of chromatographic parameters, which represents the global optimum within the limits set by the required resolution and signal-to-noise ratio specified by the user. The tolerated flow and pressure ranges, the volume of the available detector cells and the time constant of the detection system are constraints during the optimization. A separate module of the system concerns the sample preparation for pharmaceutical formulations in solid dosages and aqueous solutions. Prototype expert systems have been successfully implemented in the expert-system shell Knowledge Craft on a MicroVAX workstation.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 7
    Digitale Medien
    Digitale Medien
    Springer
    Chromatographia 28 (1989), S. 341-353 
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Diode array detectors (DAD) ; Toxicology ; Automated solute identification
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The possibilities and limitation of automated solute identification via UV/VIS spectroscopy in HPLC are demonstrated and applications in toxicologic analysis are described. A standard isocratic system is used. The influence of various chromatographic parameters on retention time is shown. A retention time window of ±15% is required. In addition to retention time, derived spectral data are calculated (minima and maxima of derivatives, area counts under standardized spectral ranges, absorption at various wavelength) and used for positive solute identification. It is possible to identify solutes with a high degree of certainty in urine and plasma if their concentration is at least 10 ppm.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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