Magnetic Resonance Spectroscopy is a technique that has the capability of measuring metabolites in vivo and, in appropriate conditions, to infer its metabolic rates. The success of MRS depends a lot on its sensitivity, which limits the usage of X-nuclei MRS. However, technological developments and refinements in methods have made in vivo heteronuclear MRS possible in humans and in small animals. This chapter provides detailed descriptions of the main procedures needed to perform successful in vivo heteronuclear MRS experiments, with a particular focus on experimental setup in ¹³ C MRS experiments in rodents.