ArticleInternational journal of molecular sciences2024
Simultaneous Determination of Enantiomeric Purity and Organic Impurities of Dexketoprofen Using Reversed-Phase Liquid Chromatography-Enhancing Enantioselectivity through Hysteretic Behavior and Temperature-Dependent Enantiomer Elution Order Reversal on Polysaccharide Chiral Stationary Phases.
Article in International journal of molecular sciences, 2024. The graph could read no effect estimate from its abstract, so it casts no vote on the map. Cited by 6 papers.
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Who cites it
6 citing papers in PubMed, 10 citations in OpenAlex.
- Enhanced Solubilization of Ketoprofen Using Triton X-100, Triton X-165, Brij C10, and Their Binary and Ternary Mixed Micelle Systems.Pharmaceutical research · 2026Article
- Chiral analysis of etomidate and metomidate enantiomers in hair by UHPLC-MS/MS: application to authentic human hair samples and enantiomeric fraction assessment.International journal of legal medicine · 2026Article
- Quantum Chemistry Based Simulation of Enantioseparation on Cyclodextrin- and Polysaccharide-Based Chiral Stationary Phases.Chemistry (Weinheim an der Bergstrasse, Germany) · 2025Article
- Article
- Possibilities and limitations of computer assisted chiral HPLC method development for ozanimod on polysaccharide based chiral stationary phases.Scientific reports · 2024Article
- Update on chiral recognition mechanisms in separation science.Journal of separation science · 2024Review
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Authors and funding
7 authors at 3 institutions in 5 countries.
Funding
Abstract
A reversed-phase high-performance liquid chromatographic (HPLC) method was developed for the simultaneous determination of the potential impurities of dexketoprofen, including the distomer R-ketoprofen. After screening the separation capability of four polysaccharide columns (Lux Amylose-1, Lux Amylose-2, Lux Cellulose-1 and Lux Cellulose-2) in polar organic and in reversed-phase modes, appropriate enantioseparation was observed only on the Lux Amylose-2 column in an acidified acetonitrile/water mixture. A detailed investigation of the mobile phase composition and temperature for enantio- and chemoselectivity showed many unexpected observations. It was observed that both the resolution and the enantiomer elution order can be fine-tuned by varying the temperature and mobile phase composition. Moreover, hysteresis of the retention times and enantioselectivity was also observed in reversed-phase mode using methanol/water mixtures on amylose-type columns. This could indicate that the three-dimensional structure of the amylose column can change by transitioning from a polar organic to a reversed-phase mode, which affects the enantioseparation process. Temperature-dependent enantiomer elution order and rare enthalpic/entropic controlled enantioseparation in the operative temperature range were also observed in reversed-phase mode. To find the best methodological conditions for the determination of dexketoprofen impurities, a full factorial optimization design was performed. Using the optimized parameters (Lux Amylose-2 column with water/acetonitrile/acetic acid 50/50/0.1 (
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Registered trials
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