Inositol phosphates are signaling molecules crucial for cellular processes. To achieve specificity, their diverse phosphorylation patterns necessitate precise molecular identification. Phosphorylation of the myo-inositol scaffold can form enantiomeric pairs, but most analysis methods only resolve regioisomers. This chapter presents an approach for enantiomer assignment using31P-NMR with l-arginine amide as a chiral solvating agent. Chemically synthesized standards enabled clear enantiomer differentiation. This method applies to both inositol phosphates as well as inositol pyrophosphates and their bisphosphonate analogs, aiding in the identification of biologically relevant isomers in natural samples.