In this work, we constructed a 13C/31P surface coil for studying cancer metabolism and bioenergetics in the brain. In a single scan session, hyperpolarized 13C-pyruvate MRS and 31P MRS were carried out for a healthy rat brain. A commercial volume proton coil was used for anatomical localization and B0 shimming. Results show good detection of 13C labeled lactate, alanine, and bicarbonate in addition to ATP, phosphocreatine, inorganic phosphate, phosphodiesters and phosphomonoesters from 31P MRS. The coil enables obtaining complementary information within a scan session, thus reducing the number of trials and minimizing biological variability for studies of metabolism and bioenergetics.