Analytical Chemistry is at the core of drug discovery and this work focuses on the use of modern techniques to study interactions of novel metallo anticancer compounds with biological targets which is crucial to better develop them. The studied compounds include supramolecular iron cylinders which should offer a new mode of binding to DNA, and steroid platinum and rhenium compounds aiming at better targeting cancer cells. In order to study these compounds interactions with DNA and proteins, a myriad of modern techniques were used including linear and circular dichroism, surface plasmon resonance, IR LASER imaging, gel electrophoresis, ESI-MS, fluorescence and UV-Vis spectroscopy. This work is a humble contribution in the very complicated quest of developing more selective anticancer compounds.