Chromatographia

, Volume 81, Issue 4, pp 719–725 | Cite as

Capillary Electrophoresis Method for the Chiral Purity Determination of Pregabalin Derivatized with Dansyl Chloride

  • Henrik Harnisch
  • Yi-han Chien
  • Gerhard K. E. Scriba
Short Communication
  • 63 Downloads

Abstract

A capillary electrophoresis method for the determination of the chiral purity of pregabalin upon derivatization with dansyl chloride was developed using design of experiment methodologies. A D-optimal design was used for the identification of the critical process parameters, while a central composite face centered design and Monte Carlo simulations were employed for defining the design space of the method. Final working conditions consisted of a background electrolyte composed of a 100 mM sodium phosphate buffer, pH 2.5, containing 40 mg mL−1 heptakis(2,3,6-tri-O-methyl)-β-cyclodextrin, a separation voltage of 15 kV and a capillary temperature of 25 °C. The analyses were carried out in a 40/50.2 cm fused-silica capillary with an inner diameter of 50 µm. Upon testing the robustness using a Plackett–Burman design, the method was validated according to the International Council on Harmonization guideline Q2(R1). The method allowed the detection of the (R)-enantiomer at the 0.015% level with a limit of quantitation at the 0.05% level with regard to a sample containing 1.59 mg mL−1 pregabalin. The method was subsequently applied to the determination of the stereochemical purity of the drug in commercial capsules.

Keywords

Pregabalin Enantiomeric purity Stereoisomer analysis Capillary electrophoresis Quality by design 

Notes

Acknowledgements

The gift of pregabalin and the racemic drug by Optimus Drugs PVT Ltd. (Hyderabad, India) is gratefully acknowledged.

Compliance with Ethical Standards

Conflict of interest

The authors have declared no conflict of interest.

Ethical approval

This article does not contain any studies with human participants or animals performed by any of the authors.

Supplementary material

10337_2018_3495_MOESM1_ESM.pdf (149 kb)
Supplementary material 1 (PDF 149 kb)

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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Henrik Harnisch
    • 1
  • Yi-han Chien
    • 1
    • 2
  • Gerhard K. E. Scriba
    • 1
  1. 1.Department of Pharmaceutical and Medicinal Chemistry, School of PharmacyFriedrich Schiller University JenaJenaGermany
  2. 2.School of Pharmaceutical SciencesWuhan UniversityWuhanChina

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