A sensitive and selective LC/MS/MS method was developed to detect diethanolamine (DEA), an impurity of toxicological concern, at part per million (ppm) levels in a pharmaceutical intermediate as part of the overall drug substance impurity control strategy.  Direct analysis of DEA using GC/MS and LC/MS was found to lack the appropriate sensitivity, linearity, and reproducibility required for accurate quantification.  A derivatization was developed to form a product that was easily and reproducibly detected by positive electrospray ionization (ESI) in the selected reaction monitoring (SRM) mode.  The DEA derivative was separated from the matrix prior to detection using a gradient and a reverse phase system.  The method was fully characterized and used successfully to evaluate several batches of intermediate.  This presentation will discuss the details of the development and characterization of this novel method used to detect DEA at ppm levels.

Using LC/MS/MS and a derivatization to detect diethanolamine at parts per million levels in a pharmaceutical intermediate

246th National Meeting (2013)

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