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  • 1.
    Lesko, Marek
    et al.
    Rzeszów University of Technology, Poland.
    Åsberg, Dennis
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Enmark, Martin
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Samuelsson, Jörgen
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Fornstedt, Torgny
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Kaczmarski, Krzysztof
    Poland.
    Choice of Model for Estimation of Adsorption Isotherm Parameters in Gradient Elution Preparative Liquid Chromatography2015Inngår i: Chromatographia, ISSN 0009-5893, E-ISSN 1612-1112, Vol. 78, nr 19-20, s. 1293-1297Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The inverse method is a numerical method for fast estimation of adsorption isotherm parameters directly from a few overloaded elution profiles and it was recently extended to adsorption isotherm acquisition in gradient elution conditions. However, the inverse method in gradient elution is cumbersome due to the complex adsorption isotherm models found in gradient elution. In this case, physicochemically correct adsorption models have very long calculation times. The aim of this study is to investigate the possibility of using a less complex adsorption isotherm model, with fewer adjustable parameters, but with preserved/acceptable predictive abilities. We found that equal or better agreement between experimental and predicted elution profiles could be achieved with less complex models. By being able to select a model with fewer adjustable parameters, the calculation times can be reduced by at least a factor of 10. 

    Fulltekst (pdf)
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  • 2.
    Olsson, Jeanette
    et al.
    Karlstads universitet, Fakulteten för teknik- och naturvetenskap.
    Marlin, Nicola D.
    Karlstads universitet, Fakulteten för teknik- och naturvetenskap.
    Blomberg, Lars G.
    Karlstads universitet, Fakulteten för teknik- och naturvetenskap.
    Enantiomeric Separation of Omeperazole Enantiomers by Aqueous CE Using UV and MS Detection2007Inngår i: Chromatographia, ISSN 0009-5893, E-ISSN 1612-1112, Vol. 66, nr 5-6, s. 421-425Artikkel i tidsskrift (Fagfellevurdert)
  • 3.
    Samuelsson, Jörgen
    et al.
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Leśko, Marek
    Rzeszow University of Technology, Rzeszow, Poland.
    Enmark, Martin
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Högblom, Joakim
    Akzo Nobel Pulp and Performance Chemicals AB.
    Karlsson, Anders
    AstraZeneca R&D.
    Kaczmarski, Krzysztof
    Department of Chemical Engineering, Rzeszow University of Technology, Rzeszow.
    Optimizing Column Length and Particle Size in Preparative Batch Chromatography Using Enantiomeric Separations of Omeprazole and Etiracetam as Models: Feasibility of Taguchi Empirical Optimization2018Inngår i: Chromatographia, ISSN 0009-5893, E-ISSN 1612-1112, Vol. 81, nr 6, s. 851-860Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The overreaching purpose of this study is to evaluate new approaches for determining the optimal operational and column conditions in chromatography laboratories, i.e., how best to select a packing material of proper particle size and how to determine the proper length of the column bed after selecting particle size. As model compounds, we chose two chiral drugs for preparative separation: omeprazole and etiracetam. In each case, two maximum allowed pressure drops were assumed: 80 and 200 bar. The processes were numerically optimized (mechanistic modeling) with a general rate model using a global optimization method. The numerical predictions were experimentally verified at both analytical and pilot scales. The lower allowed pressure drop represents the use of standard equipment, while the higher allowed drop represents more modern equipment. For both compounds, maximum productivity was achieved using short columns packed with small-particle size packing materials. Increasing the allowed backpressure in the separation leads to an increased productivity and reduced solvent consumption. As advanced numerical calculations might not be available in the laboratory, we also investigated a statistically based approach, i.e., the Taguchi method (empirical modeling), for finding the optimal decision variables and compared it with advanced mechanistic modeling. The Taguchi method predicted that shorter columns packed with smaller particles would be preferred over longer columns packed with larger particles. We conclude that the simpler optimization tool, i.e., the Taguchi method, can be used to obtain “good enough” preparative separations, though for accurate processes, optimization, and to determine optimal operational conditions, classical numerical optimization is still necessary

    Fulltekst (pdf)
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  • 4.
    Åsberg, Dennis
    et al.
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Lesko, Marek
    Leek, Tomas
    Samuelsson, Jörgen
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Kaczmarski, Krzysztof
    Fornstedt, Torgny
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Estimation of Nonlinear Adsorption Isotherms in Gradient Elution RP-LC of Peptides in the Presence of an Adsorbing Additive2017Inngår i: Chromatographia, ISSN 0009-5893, E-ISSN 1612-1112, Vol. 80, nr 6, s. 961-966Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    In electrostatic repulsive interaction chromatography, using a charged surface hybrid sorbent carrying positive charges can improve the peak shape of peptides in reversed-phase liquid chromatography (RP-LC), especially in overloaded conditions, compared with standard C-18 sorbents. However, the positive surface charges can interact with anionic additives commonly used in peptide separations, e.g., trifluoroacetic acid (TFA), complicating adsorption isotherm estimation. We investigated how the competition for available adsorption sites between TFA and two peptides influenced the adsorption isotherm in gradient elution. A model accounting for the competition with TFA was compared with a model neglecting TFA adsorption. We found that the two models predicted elution profiles with the same accuracy. We also found that the adsorption isotherms were extremely similar in shape, leading to the conclusion that neglecting the competition with TFA is a valid approximation enabling faster and more robust adsorption isotherm estimation for the studied type of sorbent.

    Fulltekst (pdf)
    fulltext
  • 5.
    Åsberg, Dennis
    et al.
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Leśko, Marek
    Rzeszów University of Technology, Poland.
    Samuelsson, Jörgen
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Karlsson, Anders
    AstraZeneca R&D Gothenburg, Mölndal.
    Kaczmarski, Krzysztof
    Rzeszów University of Technology, Poland.
    Fornstedt, Torgny
    Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper (from 2013).
    Combining Chemometric Models with Adsorption Isotherm Measurements to Study Omeprazole in RP-LC2016Inngår i: Chromatographia, ISSN 0009-5893, E-ISSN 1612-1112, Vol. 79, nr 19, s. 1283-1291Artikkel i tidsskrift (Fagfellevurdert)
    Abstract [en]

    The adsorption of the proton-pump inhibitor omeprazole was investigated using RP-LC with chemometric models combined with adsorption isotherm modelling to study the effect of pH and type of organic modifier (i.e., acetonitrile or methanol). The chemometric approach revealed that omeprazole was tailing with methanol and fronting with acetonitrile along with increased fronting at higher pH. The increased fronting with higher pH for acetonitrile was explored using a pH-dependent adsorption isotherm model that was determined using the inverse method and it agreed well with the experimental data. The model indicated that the peaks exhibit more fronting at high pH due to a larger fraction of charged omeprazole molecules. This model could accurately predict the shape of elution profiles at arbitrary pH levels in the studied interval. Using a two-layer adsorption isotherm model, the difference between acetonitrile and methanol was studied at the lowest pH at which almost all omeprazole molecules are neutral. Omeprazole had adsorbate–adsorbate interactions that were similar in strength for the acetonitrile and methanol mobile phases, while the solute–adsorbent interactions were almost twice as strong with methanol. The difference in the relative strengths of these two interactions likely explains the different peak asymmetries (i.e., tailing/fronting) in methanol and acetonitrile. In conclusion, thermodynamic modelling can complement chemometric modeling in HPLC method development and increase the understanding of the separation.

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    fulltext
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