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Updated: Mar 11, 2026

Optimization of Processing of Tiebangchui with Highland Barley Wine Based on the Box-Behnken Design Combined with the Entropy Method
Published on: May 19, 2023
Heart-cut achiral-chiral LC-LC method development using factorial design: application to the chiral separation of
Miguel Peñín-Ibáñez1, María Jesús Santos-Delgado2, Luis María Polo-Díez1
1Department of Analytical Chemistry, Faculty of Chemistry, Complutense University of Madrid, 28040, Madrid, Spain.
Abstract:
A two-dimensional achiral-chiral LC-LC method in heart-cut mode for ketoprofen and its enantiomeric fraction determination was proposed. A C8 column was used in the first dimension, and the chiral column was an α1-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.
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