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In this paper, MoS2@MIL-53(Fe) (noted as MSMF) metal–organic backbone adsorption photocatalysts were successfully prepared by a solvothermal method. For the degradation performance of MSMF catalysts on tetracycline pollutants, the effects of MoS2 doping ratio, reaction mode, and contaminant concentration on the degradation performance were investigated. And the materials were characterized by XRD, XPS, SEM, BET, PL, and ESR to investigate the reaction mechanism. The results showed that the optimal synthesis mass ratio of MoS2:MIL-53 (Fe) prepared by holding at 150 °C for 10 h was 0.20:1 (20%MSMF). In the adsorption-photocatalytic synergy experiment, 87.62% of tetracycline (30 mg/L) could be removed with 0.20 g/L of 20%MSMF after 40 min of UV irradiation, while the removal of tetracycline by MoS2 and MIL-53 (Fe) was only 35.99% and 65.40%. The characterization showed that the specific surface area and total pore volume of 20%MSMF were 1.12 and 3.12 times higher than those of MIL-53 (Fe), respectively. And the separation and transfer efficiency of electron–hole pairs were improved for 20%MSMF compared to the constituent components. These results suggest that the doping of MoS2 enhances the adsorption and photocatalytic ability of MIL-53 (Fe) that can be used for the efficient treatment of tetracycline. [ABSTRACT FROM AUTHOR]