Evaluation of three temperature- and mobile phase-dependent retention models for reversed-phase liquid chromatographic retention and apparent retention enthalpy

Horner, Anthony R.; Wilson, Rachael E.; Groskreutz, Stephen R.; Murray, Bridget E.; Weber, Stephen G.

doi:10.1016/j.chroma.2018.12.055

Cited by 11 publications

(8 citation statements)

References 39 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…CSPs, organic modifiers, and column temperature have greatly affected chiral separation of analytes . Systematic exploration for chromatographic factors will help us develop suitable conditions for analysis, determination, and preparative separation of chiral pharmaceuticals.…”

Section: Resultsmentioning

confidence: 99%

HPLC semi‐preparative separation of diclazuril enantiomers and racemization in solution

Huang

Guo

Fan

et al. 2020

J of Separation Science

View full text Add to dashboard Cite

contributed equally to this work.Diclazuril has been widely used in poultry feed for prevention and treatment of coccidiosis, and its chiral separation is rarely reported. Herein, semi-preparative separation method of diclazuril enantiomers has been developed through normal-phase high-performance liquid chromatography. Effects of chiral stationary phases, alcoholic modifiers, and column temperature on separation of diclazuril were discussed in detail. Both the single-urea-bound 4-chlorophenylcarbamoylated β-cyclodextrin and amylose tris(3,5-dimethylphenylcarbamate)-coated chiral stationary phases showed strong ability in separation of diclazuril by using n-hexane-trifluoroacetic acidethanol. Then, semi-preparative separation of diclazuril was carried out through stacked injection, and the "enantiomeric excess" purities of two fractions were over 98%. Next, the electronic circular dichroism profiles of these two fractions in ethanol solution displayed the mirror image of each other in the range 360-200 nm. Moreover, effects of acidic/basic additive, time, and temperature on racemization of diclazuril enantiomers in ethanol solution have been studied in detail through normal-phase high-performance liquid chromatography. Racemization of diclazuril enantiomers was remarkably accelerated through adding triethylamine at high temperature. We envision that this systematic investigation of diclazuril at an enantiomeric level would provide valuable information in future studies involving enantioselective bioactive, metabolic, and toxicological activities. K E Y W O R D Sdiclazuril, electronic circular dichroism spectroscopy, racemization, semi-preparative separation 1240

show abstract

Section: Resultsmentioning

confidence: 99%

HPLC semi‐preparative separation of diclazuril enantiomers and racemization in solution

Huang

Guo

Fan

et al. 2020

J of Separation Science

View full text Add to dashboard Cite

show abstract

“…The sum‐of‐squares error ( SSE ) is corrected by the number of parameters ( p ) and the number of observations ( n ). A lower (more negative) value represents a better fit, thus aiding in the selection of a correct model [15,41–45].…”

Section: Background Theorymentioning

confidence: 99%

Recent applications of retention modelling in liquid chromatography

Uijl

Schoenmakers

Pirok

et al. 2020

J of Separation Science

View full text Add to dashboard Cite

Recent applications of retention modelling in liquid chromatography (2015–2020) are comprehensively reviewed. The fundamentals of the field, which date back much longer, are summarized. Retention modeling is used in retention‐mechanism studies, for determining physical parameters, such as lipophilicity, and for various more‐practical purposes, including method development and optimization, method transfer, and stationary‐phase characterization and comparison. The review focusses on the effects of mobile‐phase composition on retention, but other variables and novel models to describe their effects are also considered. The five most‐common models are addressed in detail, i.e. the log‐linear (linear‐solvent‐strength) model, the quadratic model, the log–log (adsorption) model, the mixed‐mode model, and the Neue–Kuss model. Isocratic and gradient‐elution methods are considered for determining model parameters and the evaluation and validation of fitted models is discussed. Strategies in which retention models are applied for developing and optimizing one‐ and two‐dimensional liquid chromatographic separations are discussed. The review culminates in some overall conclusions and several concrete recommendations.

show abstract

“…For example, several groups have worked on predicting the effect of the mismatch between sample solvent and the mobile phase on peak shape and width in both one-and two-dimensional liquid chromatography (LC) [1][2][3][4]. Other groups have advanced understanding of the effect of temperature on retention in reversed-phase separations [5], worked to improve general models of retention and selectivity in RP separations [6,7], and explored the limits and implementations of retention models as a key components of method development workflows for both one-and two-dimensional LC separations [8][9][10].…”

Section: Introductionmentioning

confidence: 99%

Characterization of a High Throughput Approach for Large Scale Retention Measurement in Liquid Chromatography

Kempen

Dahlseid

Lauer

et al. 2023

Preprint

View full text Add to dashboard Cite

Many contemporary challenges in liquid chromatography - such as the need for “smarter” method development tools, and deeper understanding of chromatographic phenomena - could be addressed more efficiently and effectively with larger volumes of experimental retention data than we have been accustomed to historically. The paucity of publicly accessible, high-quality measurements has been due, at least in large part, to the high cost in time and resources associated with traditional retention measurement approaches. Recently we described an approach to improve the throughput of such measurements by using very short columns (typically 5 mm), while maintaining measurement accuracy. In this paper we present a perspective on the characteristics of results obtained using this approach using a dataset containing about 13,000 retention measurements, and describe an approach to sample introduction that improves upon the prior work. The dataset is comprised of results for 35 different small molecules, nine different stationary phases, and several mobile phase compositions for each analyte/phase combination. During the acquisition of these data, we have interspersed repeated measurements of a small number of compounds for quality control purposes. The data from these measurements not only enable detection of “out of control” measurements, but also assessment of the repeatability and reproducibility of retention measurements over time. For retention factors greater than 1, the mean relative standard deviation (RSD) of replicate (typically n=5) measurements is 0.4%, and the standard deviation of RSDs is 0.4%. Most differences between selectivity values measured six months apart for 15 non-ionogenic compounds were in the range of +/- 1%, indicating good reproducibility. A critically important observation from these analyses is that selectivity (defined here as retention of a given analyte relative to the retention of a reference compound; kx/kref) is a much more consistent measure of retention over time (months) compared to the retention factor alone. While this work and dataset also highlights the importance of stationary phase stability over time for achieving reliable retention measurements, we are nevertheless optimistic that this approach will enable the compilation of large databases (>> 10,000 measurements) of retention values over long time periods (years), which can in turn be leveraged to address some of the most important contemporary challenges in liquid chromatography. All of the data discussed in the manuscript are provided as Supplemental Information.

show abstract

Evaluation of three temperature- and mobile phase-dependent retention models for reversed-phase liquid chromatographic retention and apparent retention enthalpy

Cited by 11 publications

References 39 publications

HPLC semi‐preparative separation of diclazuril enantiomers and racemization in solution

HPLC semi‐preparative separation of diclazuril enantiomers and racemization in solution

Recent applications of retention modelling in liquid chromatography

Characterization of a High Throughput Approach for Large Scale Retention Measurement in Liquid Chromatography

Contact Info

Product

Resources

About