Abstract: There is disclosed a method for direct quantitation of total carbon and 14C/12C ratios in a single measurement using Accelerator Mass Spectrometry (AMS). More specifically, measurement of both total carbon and 14C/12C ratio is performed in the same sample at the same time. The disclosed method provides improved sensitivity and accuracy for reliably calculating 14C-labeled compound concentrations in biological samples. There is also a reduction in measurement time, sample volume requirement and measurement cost compared to existing procedures.