Uranium (U) is one of the most concerned radioactive metals on earth. Thus, to unravel the transportation and transformation of U in the food webs, and tracing its ecological and health risks are of utmost and timely importance. Radiometallomics, in conjunction with the research methods, mainly focus on establishing the ecological and biological metabolisms and behaviors of radiometals/metalloids. In particular, synchrotron radiation (SR) has many advanced properties, e.g., high brightness and collimation, and a wide energy spectrum, which make it a unique technique in the study of metal distribution and speciation analysis. To date, SR-based techniques are widely applied in the environmental sciences; however, a systematic summary of its application in radiometallomics is still lacking. This review assembled and compared the conventional and advanced techniques, especially SR-based radiometallomics used in studying U in environmental matrixes, with the aim that this information will help to develop further combined metallomics approaches in the U analysis and risk assessment of contaminated areas.