Two novel macrocycles prepared from lithocholic acid, piperazine and pyridine dicarboxylic acids (2,6- and 3,5-isomers), have been characterized by 1 3 C NMR and ESI-MS techniques. In case of the pyridine-2,6-dicarboxylate derivative, the molecular formula of the cycle was C 5 9 H 8 7 O 6 N 3 (I), while the pyridine-3,5-dicarboxylate derivative (II) was a trimeric structure by molecular mass when compared with I. Furthermore, cycle I showed a special affinity towards potassium cation, while II possessed significant proton and sodium cation recognition properties.