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  • Chemistry  (132)
  • Column liquid chromatography  (12)
  • Surface physics, nanoscale physics, low-dimensional systems
  • 1990-1994  (144)
  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Chemie in unserer Zeit 25 (1991), S. viii 
    ISSN: 0009-2851
    Keywords: Chemistry ; Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    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: 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.
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  • 4
    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.
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  • 5
    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.
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  • 6
    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.
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  • 7
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 3 Ill.
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  • 8
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The solution structure of an α-amylase inhibitor, tendamistat, calculated from nmr data with the distance geometry program DISMAN is subjected to restrained energy minimization. To study the influence of force field parametrizations and the convergence behavior of refinement algorithms, two different programs were used. AMBER is an established software package including a steepest descent and/or conjugent gradient optimizer in the Euclidian space; the name AMBER also represents a force field. The program FANTOM (fast Newton-Raphson torsion angle energy minimizer) is a new restrained energy refinement implementation of the Newton-Raphson algorithm, which uses second derivatives of the conformational energy in dihedral angle space with the ECEPP/2 force field. For both programs the normal energy force field was supplemented with an additional potential of the form ΣA(di - ui)6 (if di 〉 ui), which enforces upper limits ui to selected distances di as measured by nmr. Improvements of the intramolecular interactions with a decrease of the internal energies of about 1000 kcal/mol could be achieved without increasing the distance constraint violations. The restrained energy refinements caused only small changes of the molecular geometries: The root mean square distance values for the backbone atoms between the initial DISMAN structure and the refined structures are about 0.5 Å for AMBER and about 0.7 Å for FANTOM. Local conformational changes during the restrained energy minimizations are analyzed with respect to hydrogen-bond formation, and with respect to comparisons of the solution structure and the crystal structure.
    Additional Material: 4 Ill.
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  • 9
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Biopolymers 30 (1990), S. 975-983 
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The collective internal dynamics of transfer RNAphe from brewer's yeast in solution was studied by depolarized dynamic light scattering (DDLS). Within the melting region of tRNA the depolarized spectra consist of two Lorentzian, where the narrow (slow) component describes the overall rotation of the macromolecule. The broad component is attributed to the collective reorientation of the bases within the biopolymer. At high temperature only this relaxation process is observed in the spectrum. The viscosity dependence of the collective internal relaxation process is described by the Stokes-Einstein-Debye equation for rotational diffusion. Estimates of the internal orientational pair correlation factor from the integral depolarized intensities of tRNAPhe solutions indicates that the observed dynamics correspond to the collective reorientation of approximately 5 bases. A comparison of the results presented with DDLS studies on the aggregation of the mononucleotide guanosine-5′-monophosphate confirms this result. For a further characterization of the relaxation process we studied the effect of hydrostatic pressure (1-1000 bar) on the depolarized spectra of tRNA. While other spectroscopic methods like nmr, fluorescence polarization anisotropy decay, or ESR give information about the very local motion of a single base within the DNA or RNA, this study shows that by DDLS one can characterize collective internal motions of macromolecules.
    Additional Material: 3 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Biopolymers 31 (1991), S. 813-825 
    ISSN: 0006-3525
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Photon correlation spectroscopy has been used to study the translational (D0)and internal dynamics of monodisperse linear and polydisperse superhelical plasmid-DNAs. Scattering vector dependent correlation functions were measured and analyzed with the inverse Laplace transform CONTIN written by S. Provencher. For scattering vectors (q) lower than 1.3 × 105cm-1, D0 can be separated from internal dynamics. Using the measured D0value, the q dependence of internal modes was determined. Extrapolation of the internal relaxation times for q → 0 yields the longest internal relaxation time t1. This time can be connected to the persistence length in terms of the Berg-Soda model, which describes the molecule as a semiflexible circular polymer with hydrodynamic interactions. The calculated length of 76 nm for DNA, I = 0.15 mol/L, is a little higher than the one obtained from static light scattering data without excluded volume corrections. A comparison of experimental and simulated correlation functions for the Berg-Soda model shows that the model gives a fairly good description of the dynamics of the linear molecule, whereas large discrepancies between model and experimental functions are observed for the superhelical DNA. Small differences between model and experimental functions are mainly attributed to the neglect of the torsional modes that may be coupled to bending and flexing modes. For the superhelical DNA the agreement is improved if the calculation is carried out with a linear molecule, with shorter contour length and increased diameter. Both quantities can be derived from the known superhelix tilt angle.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
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