Chromatographia

, Volume 44, Issue 7–8, pp 355–361 | Cite as

Improvements in drug purity determination by capillary electrophoresis using UV-absorption and LIF-detection with a UV-laser

  • O. Stålberg
  • D. Westerlund
  • U-K. Hultin
  • S. Schmidt
Originals

Summary

In drug purity determinations by capillary electrophoresis using UV-detection generally a relative high concentration of the main compound has to be injected. Principles how to handle overloading effects are described. NXX-066 is a drug with a native fluorescence which made it possible to use of CE system equipped with a LIF-detection unit. Monitoring drug purity determination with LIF detection results in an improved limit of quantification of the impurities and/or opens a possibility to avoid an overloaded main peak. A frequency doubled (FRED) argon ion laser set at 244 nm was used as excitation source in drug purity determination with the LIF-detection unit and the chemicals used were therefore carefully chosen in order to minimize the background noise level, which easily is enhanced when fluorescence detection is performed in the UV-range. The separation of the fluorescent NXX-066 analogues proved to be a difficult task, but an adequate resolution was obtained when β- and γ-cyclodextrins was added as structural selectors and the separation window was expanded by the use of a repressed/reversed electroosmotic flow. A comparison of the separation capability for the UV-detection system and the laser induced fluorescence detection system was performed, showing that the overloading effects of the main peak can be removed using the CE-LIF system and thereby obtain a substantially improved resolution of the analogues. A comparison of LC-UV and CE-UV for drug purity determination of a crude product from, synthesis of NXX-066 is also included in this paper where a good correlation of the results were obtained.

Key Words

Capillary electrophoresis Drug purity Frequency doubled laser Laser induced fluorescence Reduced electromigration dispersion 

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Copyright information

© Friedr. Vieweg & Sohn Verlagsgesellschaft mbH 1997

Authors and Affiliations

  • O. Stålberg
    • 1
  • D. Westerlund
    • 1
  • U-K. Hultin
    • 2
  • S. Schmidt
    • 2
  1. 1.Analytical Pharmaceutical ChemistryUppsala University Biomedical CentreUppsalaSweden
  2. 2.Astra Arcus AB, Analytical and Pharmaceutical R & DSödertäljeSweden

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