Robust UHPLC separation method development for multi-API product containing amlodipine and bisoprolol: The impact of column selection

Róbert Kormány, Imre Molnár, Jeno Fekete, Davy Guillarme, Szabolcs Fekete

Research output: Contribution to journalArticle

16 Citations (Scopus)

Abstract

This paper describes a new and fast ultra-high pressure liquid chromatographic separation of amlodipine and bisoprolol and all their closely related compounds, for impurity profiling purposes. Computer-assisted method development was applied and the impact of several state-of-the-art stationary phase column chemistries (50 x 2.1 mm, sub-2 μm, and core-shell type materials) on the achievable selectivity and resolution was investigated. The work was performed according to quality by design principles using design of experiment with three experimental factors; namely the gradient time (t G), temperature (T), and mobile phase pH. Thanks to modeling software, it was proved that the separation of all compounds was feasible on numerous column chemistries within <10 min, by proper adjustments of variables. It was also demonstrated that the reliability of predictions was good, as the predicted retention times and resolutions were in good agreement with the experimental ones. The final, optimized method separates 16 peaks related to amlodipine and bisoprolol within 7 min, ensuring baseline resolution between all peak-pairs.

Original languageEnglish
Pages (from-to)1119-1127
Number of pages9
JournalChromatographia
Volume77
Issue number17-18
DOIs
Publication statusPublished - Jan 1 2014

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Keywords

  • Amlodipine
  • Bisoprolol
  • DryLab
  • Method development
  • Quality by design (QbD)
  • UHPLC

ASJC Scopus subject areas

  • Analytical Chemistry
  • Biochemistry
  • Clinical Biochemistry
  • Organic Chemistry

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