I wouldn't expect a different concentration of Tc in this instance, unless the assumption is that the urine excreted is more concentrated than normal. I wouldn't predict that change.
An aliquot of urine could easily be counted in a well-type scintillation counter using proper counting methodology
In animal study you should separate urinary bladder and count its radioactivity in a well type counter, but in clinical study you can use from urine counting or direct count with SPECT Detector.
I am interested in the free TcO4 and the intact complex because I want to determine whether addition of MDP has an effect on biological and effective half life of Tc
The ratio of intact product to free Tc may be easily determined by chromatography as described by the United States or any other Pharmacopeia. Paper TLC using acetone or silica gel using saline are commonly used for this purpose.