The preparation and the structural characterization of two La(III)-based coordination polymers was described in this study, in which {[La(H2O)(BTCTB)]·2H2O}n (1, H3BTCTB = 3,3′,3′′-[1,3,5‐benzenetriyltris(carbonyl amino)] three benzoic acid) and [(La2(TATAB)2)·4DMF·4H2O]n (2, H3TATAB = 4,4,4″s-triazine-1,3,5-triethyl-m-aminobenzoic acid) were prepared by means of two flexible tricarboxylic acid ligands with different joints and functional backbones. Moreover, a sonochemical synthesis way has been carried out to produce the nanostructures of complexes 1 and 2. In addition, their anticancer activity was evaluated on nasopharyngeal carcinoma cells. Firstly, Cell Counting Kit-8 test kit was used to test the cancer cells proliferation after treated with nano 1 or 2. Then, the Annexin V-FITC/PI test was performed and the percentage of the apoptotic cancer cells was determined after nano 1 and 2 treatment. Next, the ROS accumulation after nano 1 and 2 treatment was detected by DCFH-DA detection kit. Finally, the expression level of FHIT in nasopharyngeal carcinoma cells treated with nano 1 and 2 was evaluated via western blot.