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Analytical and Bioanalytical Chemistry

, Volume 401, Issue 4, pp 1365–1375 | Cite as

Identification and characterization of impurities of tetracosactide by capillary electrophoresis and liquid chromatography coupled to time-of-flight mass spectrometry

  • Angelina Taichrib
  • Gerhard K. E. Scriba
  • Christian Neusüß
Original Paper

Abstract

Tetracosactide is a synthetic peptide analogue of the human adrenocorticotropic hormone that stimulates the production of cortisol in the adrenal cortex. The medical use of the compound is primarily the diagnosis of the adrenal cortex function. In order to characterize impurities of the drug, tetracosactide samples were analysed by both liquid chromatography and capillary electrophoresis coupled to a quadrupole time-of-flight mass spectrometer. The identification of the impurities was carried out based on accurate mass determination and fragment ion spectra. The presence of several peptides of lower and higher masses than tetracosactide could be shown, including N- and C-terminally truncated peptides as well as peptides which still contained protecting groups or additional amino acids. Furthermore, a semi-quantitative estimation of the relative amounts of the impurities in different samples as well as a commercial preparation revealed that the number and the type of the impurities varied between the samples. Comparing the selectivity of liquid chromatography and capillary electrophoresis regarding the separation of tetracosactide impurities, it can be stated that capillary electrophoresis showed a higher suitability for the separation of tetracosactide fragments (smaller peptides) while the larger peptides, i.e. those wearing protecting groups, were separated more efficiently by liquid chromatography.

Keywords

Tetracosactide Impurity identification LC/MS CE/MS 

Notes

Acknowledgements

The Federal Institute for Drugs and Medical Devices (BfArM, Bonn, Germany) is gratefully acknowledged for providing the samples of TCS and its impurities. AT thanks the Thomas Gessmann Foundation for financial support.

Supplementary material

216_2011_5183_MOESM1_ESM.pdf (1.1 mb)
Table S1 (PDF 1.10 mb)

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Copyright information

© Springer-Verlag 2011

Authors and Affiliations

  • Angelina Taichrib
    • 1
  • Gerhard K. E. Scriba
    • 2
  • Christian Neusüß
    • 1
  1. 1.Chemistry DepartmentAalen UniversityAalenGermany
  2. 2.Department of Pharmaceutical ChemistryFriedrich Schiller University JenaJenaGermany

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