Research into the areas of synchrotron generated microbeam radiotherapy (MRT) and stereotactic radiosurgery is increasing. Such MRT techniques are showing potential of tackling some of the more difficult radiotherapy cases such as certain type of brain tumours. Two challenging aspects of these techniques are addressed in this investigation; the difficulty of dose determination and the delivery of the treatments at lower dose levels. In this research polymer gels were used as phantoms and dosimeters and cells were used to confirm outcomes. Normoxic polyacrylamide gels (nPAG) were tested as potential dosimeters for microbeam dosimetry. Following irradiation using microbeam and minibeam radiation from the BL28BU beam-line at Spring-8, Japan, the nPAG were scanned using a Raman spectroscopy technique. Dose enhancement caused by the inclusion of the gold nanoparticles (AuNPs) in the target was investigated using both cells and polymer gels. The use of AuNP could potentially reduce the dose required for the delivery of MRT. In this study it was shown that using endothelial cells with AuNPs, the minimal dose for clear cell killing along the beam line was reduced to 10 Gy. Both studies cell and gel studies indicates significant dose enhancement caused by the gold atoms in the target.