A two-dimensional achiral-chiral LC-LC method in heart-cut mode for ketoprofen and its enantiomeric fraction determination was proposed. A C column was used in the first dimension, and the chiral column was an α-acid glycoprotein. The mobile phase of the chiral system was optimized by a factorial design. The effect of temperature on retention and on enantiomeric resolution was studied. Particular attention was paid to mobile phase compatibility for the two columns and to transferring time, using ketoprofen standards. The R-(-) and S-(+)-ketoprofen retention times were 9 and 11 min, respectively; the resolution was higher than 1.1 and enantiomeric fraction close to 0.5. The method was applied to capsules and gels containing ketoprofen. Factorial design was also used to establish the best conditions for gel sample preparation. Recoveries were 84 and 105 % for capsules and gels, respectively. Graphical abstract Two-dimensional chromatogram for KPF and its enantiomers.
Profens are important non‐steroidal anti‐inflammatory pharmaceutical drugs and their behavior depends on their enantiomeric form. Three of the most employed profens, ketoprofen, naproxen and ibuprofen, were separated simultaneously in pairs by two‐dimensional achiral‐chiral high‐performance liquid chromatography using heart‐cut mode. The total amount of each profen was determined using a C8 column in the first achiral system; in the second chiral system, the enantiomeric fraction of each profen was determined using an α1‐acid glycoprotein column. Mobile phases were optimized by factorial design, response surfaces and multi‐response analysis paying particular attention to mobile phase compatibility of both columns and to transferring time between systems. The effect of temperature on each profen and their enantiomer retention was studied, the thermodynamic parameters being calculated. Calibration graphs were linear in the ranges of 2–20, 0.5–10 and 10–40 mg/L for ketoprofen, naproxen and ibuprofen respectively in both systems. The method allowed the analysis of three pharmaceuticals establishing the enantiomeric fraction of each profen using a simple sample preparation; moreover, the first achiral system cleans the sample deeply preventing deterioration of the expensive chiral column. Recoveries over 80% and the enantiomeric fraction of each profen were obtained allowing determination of the pharmaceutical purity.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.
hi@scite.ai
10624 S. Eastern Ave., Ste. A-614
Henderson, NV 89052, USA
Copyright © 2024 scite LLC. All rights reserved.
Made with 💙 for researchers
Part of the Research Solutions Family.