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Identification and Characterization of Tetracosactide Impurities by CE and RP-HPLC coupled to TOF MS

Sep. 14, 2011
Identification and Characterization of Tetracosactide Impurities by CE and RP-HPLC coupled to TOF MS
Identification and Characterization of Tetracosactide Impurities by CE and RP-HPLC coupled to TOF MS more

The peptide tetracosactide (TCS) is a synthetic analogue to human adrenocorticotropic hormone which stimulates the production of cortisol in the adrenal glands. It is applied pharmaceutically for the diagnosis of adrenal cortex dysfunction.

Routine analyses by RP-HPLC with UV-detection revealed several peaks (partially) separated from TCS that couldn't be associated with known impurities (TCS sulfoxide or the D-16Lysdiastereomer). For the identification of these impurities both RPHPLC and CE coupled to a QTOF MS were applied. Hence, the unknown impurities could be identified by means of accurate mass determination and fragment ion spectra. The selectivity of RP-HPLC and CE regarding the separation of these impurities is discussed. Furthermore, samples from two different suppliers and
a pharmaceutical preparation were compared.

Conclusions

  • In combination with efficient separation by CE or RP-HPLC QTOF MS is a suitable technique for the identification of unknown impurities
  • Identified impurities covered N- and C-terminally truncated peptides, peptides with additional amino acids, and peptides with residual protecting groups
  • migration times are strongly influenced by charge, whereas retention times stronger depend on hydrophobicity of analytes

- CE shows a higher suitability for the separation of TCS fragments (smaller peptides)

- larger peptides (e.g. with residual protecting groups) are separated more efficiently by RP-HPLC

  • Similar impurities were found in TCS samples from different suppliers; however the relative amounts differed considerably.

 

Angelina Taichrib1, Gerhard Scriba2, Christian Neusüß1

1 Aalen University, Chemistry Department, christian.neuseuess@htw-aalen.de

2 Friedrich Schiller University Jena, Department of Pharmaceutical Chemistry

 

This poster was presented at HPLC 2011, 19 - 23 June in Budapest, Hungary.

Please click here to read the poster as a PDF

 

 

 

Authors:
Angelina Taichrib
Gerhard Scriba
Christian Neusüß

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Keywords : Aalen University Angelina Taichrib Christian Neusüß Chromatography Friedrich Schiller Gerhard Scriba HPLC 2011 HPLC 2011 Poster identification of unknown impurities Mass Specrtometry Pharma Poster Poster HPLC RP-HPLC Screening Science Separation TOF MS University Jena

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