Profiling indomethacin impurities using high-performance liquid chromatography and nuclear magnetic resonance

Eur J Pharm Sci. 2001 Dec;14(4):301-11. doi: 10.1016/s0928-0987(01)00198-1.

Abstract

The anti-inflammatory drug indomethacin was investigated regarding new related impurities. Therefore, related substances 2-9 were prepared by independent synthesis and physicochemically characterized. To determine indomethacin and its related substances, a new HPLC-UV method was developed and validated. Indomethacin and its impurities were eluted on a C(18) column with a mobile phase consisting of methanol and an aqueous solution of 0.2% phosphoric acid at a flow rate of 1.5 ml/min and were quantified by UV detection at 320 nm. Overall, the HPLC-UV method was simple and reliable for the detection of eight impurities in indomethacin. In addition to the HPLC-UV method, 1H nuclear magnetic resonance (NMR) was used to investigate indomethacin regarding impurities. For that purpose, related substances 2-9 were systematically added to indomethacin and investigated. The NMR method was found to be very useful for the identification of impurities in bulk substance without prior separation. Both HPLC-UV and NMR were used to analyze 38 batches of indomethacin available on the European market. The outcome was that 42% of the batches did not meet the compendial requirements although they met the specifications of current compendial methods. Some batches contained the previously undescribed impurity 8, while other batches contained by-products from two distinct synthetic routes. The methods presented herein are important contributions to the ongoing efforts to reduce impurities and therefore the risk of adverse side-effects in drugs that are no longer under patent protection.

Publication types

  • Research Support, Non-U.S. Gov't
  • Validation Study

MeSH terms

  • Anti-Inflammatory Agents, Non-Steroidal / analysis*
  • Anti-Inflammatory Agents, Non-Steroidal / isolation & purification*
  • Chromatography, High Pressure Liquid / standards
  • Indomethacin / analysis*
  • Indomethacin / chemical synthesis
  • Indomethacin / isolation & purification*
  • Nuclear Magnetic Resonance, Biomolecular / methods
  • Protons
  • Reproducibility of Results
  • Spectrophotometry, Ultraviolet / standards

Substances

  • Anti-Inflammatory Agents, Non-Steroidal
  • Protons
  • Indomethacin