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Updated: May 24, 2026

Quantifying X-Ray Fluorescence Data Using MAPS
Published on: February 17, 2018
Applicability of total reflection X-ray fluorescence (TXRF) as a screening platform for pharmaceutical inorganic
Bradley J Shaw1, David J Semin, Michael E Rider
1Analytical Research and Development, Amgen Inc., One Amgen Center Drive, Thousand Oaks, CA 91320, USA. bshaw@amgen.com
Abstract:
Palladium (Pd) is extensively used in pharmaceutical small molecule drug substance processes, however it must be removed prior to release of the active pharmaceutical ingredient (API). Evaluation of four TXRF instruments and configurations were compared to ICP-MS instrumentation for trace metal analysis, most importantly for Pd. Standards and six pharmaceutical drug substances, triprolidine HCl, diphenhydramine HCl, chlorpheniramine maleate, pseudoephedrine HCl, ephedrine sulfate, and scopolamine HBr, were analyzed to determine linearity, sensitivity, accuracy, and precision for Pd plus Cr, Fe, Cu, Rh, and Pt versus interferences, particularly from Cl, S, and Ar, on the various X-ray fluorescence lines. Irrespective of instrument platform, in general X-ray sources capable of accessing Pd-K lines were found to be most effective in determination of Pd in APIs.
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