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Accelerator mass spectrometry (AMS) is an ultra-sensitive analytical method suitable for the detection of sub-nM concentrations of labeled biological substances such as pharmaceutical drugs in body fluids. A limiting factor in extending the concentration measurements to the sub-pM range is the natural 14C content in living tissues. This was circumvented by separating the labeled drug from the tissue matrix, using standard high-performance liquid chromatography (HPLC) procedures.