A new Zn(II) metal–organic framework of [Zn6(L)3(DMA)4]·5DMA (1) (H4L = [1,1′:3′,1″-terphenyl]-3,3″,5,5″-tetracarboxylic acid), was used as a drug carrier of 5-fluorouracil (5-FU) for drug delivery. Drug release behavior was also investigated under different pH condition. 5-FU is released in a highly controlled and progressive manner with 95.8% of the drug release after 96 h at acidic condition and with 91.6% after 96 h at PBS. Vitro cytotoxicity assays indicated that the 1 possesses no obvious cytotoxicity.