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Chromatographic Parameters (chromatographic + parameter)
Selected AbstractsDetermination of lipophilic descriptors of antihelmintic 6,7-diaryl-pteridine derivatives useful for bioactivity predictionsBIOMEDICAL CHROMATOGRAPHY, Issue 6 2003Mario Reta Abstract The liquid chromatographic retention factors extrapolated to pure water, k,w, for several 6,7-diaryl-pteridine derivatives in both an octadecylsilane (ODS) and an immobilized arti,cial membrane column (IAM.PC.DD2), using acetonitrile,aqueous buffer pH = 7.45 as mobile phase, were obtained. The logarithms of the k,w values in the IAM.PC.DD2 column, log k,wIAM, show good correlation with the calculated values of the octanol,water partition coef,cients, log Po/w, showing that the chromatographic parameter can be used as lipophilicity descriptor for the studied pteridines. However, interactions other than the lipophilic ones seem to be involved in the ODS column. Previous studies have shown that pteridines have antihelmintic properties. In spite of the complexity of the studied biological system as compared with the chromatographic one, good correlation between the descriptors obtained in the IAM column and biological activity (expressed as the log of the inhibitory concentration required to obtain up to 50% in the reduction of population growth of nematodes, log IC50) was observed. Copyright © 2003 John Wiley & Sons, Ltd. [source] Highly cross-linked polymeric capillary monoliths for the separation of low, medium, and high molecular weight analytesJOURNAL OF SEPARATION SCIENCE, JSS, Issue 15-16 2009Said H. Lubbad Abstract Highly rigid capillary monoliths with low swelling propensity were prepared within the confines of 200 ,m ID fused silica capillaries via thermally induced free radical polymerization of tetrakis(4-vinylbenzyl)silane (TVBS) in the presence of 1-dodecanol and toluene. ,,,,-Azobisisobutyronitrile (AIBN) was used as initiator. The resulting monoliths were optimized for the separation of low, medium, and high molecular weight analytes. The microstructure and porosity of the monoliths prepared were studied by SEM and inverse size-exclusion chromatography (ISEC). The porosity of the monolithic supports was tuned by varying the amount of initiator (i. e. AIBN) between 0.5 and 2 wt%. All monoliths were tested for a series of low molecular weight compounds including alkylbenzenes, amines, carboxylic acids, phenols, carbonyl compounds, and ,-blockers, as well as for the separation of medium molecular weight analytes such as peptides and high-molecular weight analytes such as proteins. Due to the microporous structure, the novel monoliths displayed high efficiency and performance particularly in the separation of low molecular weight analytes. Relevant chromatographic parameters including permeability, swelling propensity, and height equivalents to theoretical plates were determined. [source] Chiral analysis of milnacipran by a nonchiral HPLC , circular dichroism: Improvement of the linearity of dichroic response by temperature controlJOURNAL OF SEPARATION SCIENCE, JSS, Issue 16-17 2008Marie Lecoeur-Lorin Abstract The determination of the enantiomeric excess (e.e.) of a basic drug has been investigated in LC using a nonchiral stationary phase and a circular dichroism (CD) detector in order to avoid expensive chiral columns. The CD detector records both dichroic (,,) and UV (,) signals at the same wavelength and calculates the anisotropy factor (g = ,,/,), which is linearly related to the e.e. The enantiomeric and chemical composition of a chiral drug can be simultaneously determined on a nonchiral HPLC support. However, the g factor from the CD signal is temperature dependent. Indeed, the temperature has an influence on the stability of the CD signal and the linear regression between g factor and the e.e. of 1R,2S -enantiomer. So, a decrease in temperature gives rise to an improvement of the above-mentioned linearity correlation. After optimization of chromatographic parameters (porous graphitic carbon-based column, methanol/ phosphate buffer as mobile phase) and selection of CD wavelength, a linear regression of g factor versus e.e. of 1R,2S -enantiomer was obtained at temperature-controlled CD detection and an LOQ of 94% was found. The enantiomeric composition of milnacipran was determined with good accuracy. [source] Investigation of factors influencing the performance of open-tubular stationary phases in capillary electrochromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 9-10 2003Ruth Freitag Abstract Silica-based, open-tubular capillary columns bearing C8-moieties were produced by the sol gel approach. The influence of experimental conditions adjusted during the preparation of the stationary phase on the performance of the resulting capillary column were investigated in terms of the plate height, the resolution, and the capacity factors, taking the separation of three non-charged polyaromatic hydrocarbons (naphthalene, phenanthrene, pyrene) as example. Acetone served as EOF marker. The optimal synthesis protocol was then used to prepare columns for an analogous investigation of the chromatographic parameters, namely the mobile phase composition, the applied voltage and temperature, as well as the column length, thickness, and inner diameter on the performance of the capillary columns. [source] Studies on azaspiracid biotoxins.RAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 24 2002In this study, the performance of monolithic columns was evaluated for ultrafast liquid chromatography/mass spectrometry (LC/MS) analyses and for high-resolution separations of several azaspiracid biotoxin analogs. Because of their high permeability, monolithic columns offer a number of advantages over conventional packed columns; viz., very low backpressures and relatively flat van Deemter curves at high flow rates. That is, very high flow rates can be used for ultrafast analyses or, by using longer than normal columns, high-resolution separations are possible. In a series of experiments, we varied the mobile phase flow rates between 1 and 8,mL/min, and studied their impact on chromatographic parameters such as retention time, resolution, number of plates and pressure. The chromatographic run times could be reduced to ca. 30,s without a significant change in the separation efficiency. A signal intensity comparison revealed interesting differences between atmospheric-pressure chemical ionization (APCI) and electrospray ionization (ESI) in their flow-rate dependency. An explanation with respect to the behavior as of a mass-flow or a concentration-dependent device is given in the paper. Additionally, the column length was varied between 10 and 70,cm. As a result, the number of theoretical plates increased substantially. In the example shown in the report, an increase from 13,000 plates for a 10-cm column to 80,000 for a 70-cm column is demonstrated. In addition, the potential of the monolithic columns for high-resolution LC/MS separations is shown for a complex biotoxin mixture, which was separated on a 40-cm-long column. Copyright © 2002 John Wiley & Sons, Ltd. [source] | ||||||||||