Proton activation analysis has been recently applied for the determination of stable isotopes of trace metals in blood plasma samples taken from volunteers during tracer kinetic studies. The very low values of intestinal uptake for some elements, like ruthenium, make the kinetics of the excretion crucial for interpreting the bioassay data. Therefore, a procedure has been developed to process urine samples in order to have proper targets for the activation with protons. Preliminary tests with Ru-doped samples, conducted using the MC-40 Cyclotron at JRC Ispra, has confirmed the feasibility of the method. The minimum detectable concentrations, in the current operating conditions, are 16 ng 99Ru·ml−1 and 0.5 ng 101Ru·ml−1.