Highlighting Important Parameters Often Neglected in Numerical Optimization of Preparative Chromatography

Samuelsson, Jörgen; Enmark, Martin; Forssén, Patrik; Fornstedt, Torgny

doi:10.1002/ceat.201100210

Cited by 18 publications

(7 citation statements)

References 23 publications

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“…The reason why the peak shapes of the neutral compounds is more symmetrical than those of ionizable compounds is that their binding constant on these “active” sites is much smaller than that experienced by the ionizable compounds for comparable retention factors. Indeed, the elution of ions requires always a larger amount of water in the eluent than that necessary to elute neutral chemicals .…”

Section: Resultsmentioning

confidence: 99%

Hydrophilic interaction chromatography: A promising alternative to reversed‐phase liquid chromatography systems for the purification of small protonated bases

Gritti

Guiochon

2015

J of Separation Science

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The overloaded band profiles of the protonated species of propranolol and amitriptyline were recorded under acidic conditions on four classes of stationary phases including a conventional silica/organic hybrid material in reversed-phase liquid chromatography mode (BEH-C18), an electrostatic repulsion reversed-phase liquid chromatography C18 column (BEH-C18+), a poly(styrene-divinylbenzene) monolithic column, and a hydrophilic interaction chromatography stationary phase (underivatized BEH). The same amounts of protonated bases per unit volume of stationary phase were injected in each column (16, 47, and 141 μg/cm(3)). The performance of the propranolol/amitriptyline purification was assessed on the basis of the asymmetry of the recorded band profiles and on the selectivity factor achieved. The results show that the separation performed under reversed-phase liquid chromatography like conditions (with BEH-C18, BEH-C18+, and polymer monolith materials) provide the largest selectivity factors due to the difference in the hydrophobic character of the two compounds. However, they also provide the most distorted overloaded band profiles due to a too small loading capacity. Remarkably, symmetric band profiles were observed with the hydrophilic interaction chromatography column. The larger loading capacity of the hydrophilic interaction chromatography column is due to the accumulation of the protonated bases into the diffuse water layer formed at the surface of the polar adsorbent. This work encourages purifying ionizable compounds on hydrophilic interaction chromatography columns rather than on reversed-phase liquid chromatography columns.

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Section: Resultsmentioning

confidence: 99%

Hydrophilic interaction chromatography: A promising alternative to reversed‐phase liquid chromatography systems for the purification of small protonated bases

Gritti

Guiochon

2015

J of Separation Science

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“…The rectangular injection profiles have been employed in the calculation for the sake of simplicity. Although the use of real injection profiles would give us slightly more accurate results of the isotherm parameters, this would generate much complexity in the simultaneous fitting of the isotherm parameters because the injection profiles become more eroded with the increasing flow rates and size of the solute . The error generated from the simplified injection profiles is maximum 2–3% , which is acceptable in this case.…”

Section: Modelingmentioning

confidence: 99%

Chromatographic resolution and isotherm determination of (R,S)‐mandelic acid on Chiralcel‐OD column

Mao

Zhang

Rohani

et al. 2012

J of Separation Science

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Resolution of racemic mandelic acid ((R,S)-MA) and numerical determination of binary competitive isotherm of (R,S)-MA on Chiralcel-OD column have been investigated in this study. The effects of the alcohol modifier and acidic additive in the mobile phase on the retention and enantioseparation of (R,S)-MA were studied at first. The inverse method was then used to determine the competitive isotherm parameters of (R,S)-MA by minimizing the sum of square deviations of the model predictions from the measured elution profiles. The results indicate that the mobile phase with 85% hexane/15% isopropanol/0.3% trifluoroacetic acid mixture gives the best resolution of (R,S)-MA and competitive-modified Langmuir isotherm provides the more accurate sorption mechanism of (R,S)-MA on the cellulose tris(3,5-dimethylphenylcarbamate) chiral stationary phase.

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“…Easily reproducible fundamental studies in LC can be done using integrated commercially available system provided that the accuracy of delivered volumetric flow, the temperature control and the system void volumes are properly verified [8,15]. However, in a recent study it was shown that, in order to have reproducible experiments using commercially available system SFC systems, additional sensors are needed to measure the mass flow and the pressure at the column inlet and outlet [9].…”

Section: Introductionmentioning

confidence: 98%

Determination of adsorption isotherms in supercritical fluid chromatography

Enmark

Forssén

Samuelsson

et al. 2013

Journal of Chromatography A

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Highlighting Important Parameters Often Neglected in Numerical Optimization of Preparative Chromatography

Cited by 18 publications

References 23 publications

Hydrophilic interaction chromatography: A promising alternative to reversed‐phase liquid chromatography systems for the purification of small protonated bases

Hydrophilic interaction chromatography: A promising alternative to reversed‐phase liquid chromatography systems for the purification of small protonated bases

Chromatographic resolution and isotherm determination of (R,S)‐mandelic acid on Chiralcel‐OD column

Determination of adsorption isotherms in supercritical fluid chromatography

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