May 15–17, 2007, ACD/Labs 5^th Annual United Kingdom Users' Meeting, Old Windsor, UK

Databasing of NMR Data Benefits Impurities & Degradants Research

Steve Coombes

Abstract

Pharmaceutical Research & Development is one of the most highly regulated industries with strict controls on sample purity and the control of any potentially hazardous related materials. As such, the levels of impurities present in the Active Pharmaceutical Ingredient (API) and degradants present in the Drug Product (DP) must be identified and controlled at predefined limits.

The identification of these impurities and degradants is achieved through a combination of separation science and spectroscopy. Typical approaches include HPLC-UV, Mass Spectrometry and NMR Spectroscopy (including LC-MS and LC NMR-MS). The spectroscopic data is then analysed and interpreted in order to identify the structures of the compounds of interest.

Many software tools are available to help with the processing and analysis of spectroscopic data and herein we discuss the use of assignment and spectral databases for improved Knowledge Management; enabling global information sharing, helping to avoid duplication of analysis and improving the productivity of data analysis.

We will describe how databasing assigned ¹H and ¹³C NMR data into proprietary assignment databases can lead to the improved accuracy of predicted NMR spectra for "unknown" structures. Also, we show that the use of spectral databases can help rapidly establish how the structure of an unidentified impurity differs from or is consistent with that of the parent compound. Additionally, we describe how Computer Assisted Structure Elucidation (CASE) can be used to identify the structures of unknown impurities and how utilising the information in assignment databases can increase the efficiency of this process.

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