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Heart-cut achiral-chiral LC-LC method development using factorial design: application to the chiral separation of ketoprofen

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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.

Two-dimensional chromatogram for KPF and its enantiomers

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Acknowledgment

The present work received financial support from Project 152GR10581, supported by Complutense University of Madrid (Spain).

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Authors and Affiliations

  1. Department of Analytical Chemistry, Faculty of Chemistry, Complutense University of Madrid, 28040, Madrid, Spain

    Miguel Peñín-Ibáñez, María Jesús Santos-Delgado & Luis María Polo-Díez

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  1. Miguel Peñín-Ibáñez
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  2. María Jesús Santos-Delgado
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  3. Luis María Polo-Díez
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Correspondence to María Jesús Santos-Delgado.

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Peñín-Ibáñez, M., Santos-Delgado, M.J. & Polo-Díez, L.M. Heart-cut achiral-chiral LC-LC method development using factorial design: application to the chiral separation of ketoprofen. Anal Bioanal Chem 409, 1135–1144 (2017). https://doi.org/10.1007/s00216-016-0039-2

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