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Local recurrence has become the main problem of tumor thermal ablation for hepatocellular carcinoma (HCC). Nanotechnology could potentially aid in improving the situation. MoS₂ nanomaterials, as ideal photothermal therapy (PTT) agents, have gathered great interest due to their excellent surface plasmon resonance features, high photothermal conversion efficiency, good biocompatibility and low cost. In this work, we synthesized layered MoS₂ hollow spheres (LMHSs; diameter ∼300 nm) via the solvent-controlled ultrasonic nebulization method. Compared to LMHSs previously synthesized by our group (approx. 600 nm), the current ones showed better efficacy, as well as enhanced permeability and retention, due to their ideal size. In addition, the LMHSs are developed with both layered and hollow structures, which are extremely suitable for loading anticancer agents. In this study, doxorubicin (DOX) was loaded into the nanoparticles (NPs) using the vacuum negative pressure loading method, and the drug loading capacity was as high as 32.5%. Therefore, the efficacy of cancer cell killing by photothermal ablation was markedly enhanced by DOX released from the LMHSs. As we expected, the as-made DOX@MoS₂ NPs exhibited excellent photothermo-chemotherapy effect, both in vitro and in vivo. Tumor cell viability was inhibited up to 73% at the power density of 1.2 W cm-2, and tumors in mice models achieved complete response, with no recurrence. The PTT with DOX@MoS₂ NPs had a much better synergistic therapeutic efficacy than each individual treatment, showing great promise for HCC treatment.

Local recurrence has become the main problem of tumor thermal ablation for hepatocellular carcinoma (HCC). Nanotechnology could potentially aid in improving the situation. MoS₂ nanomaterials, as ideal photothermal therapy (PTT) agents, have gathered great interest due to their excellent surface plasmon resonance features, high photothermal conversion efficiency, good biocompatibility and low cost. In this work, we synthesized layered MoS₂ hollow spheres (LMHSs; diameter ∼300 nm) via the solvent-controlled ultrasonic nebulization method. Compared to LMHSs previously synthesized by our group (approx. 600 nm), the current ones showed better efficacy, as well as enhanced permeability and retention, due to their ideal size. In addition, the LMHSs are developed with both layered and hollow structures, which are extremely suitable for loading anticancer agents. In this study, doxorubicin (DOX) was loaded into the nanoparticles (NPs) using the vacuum negative pressure loading method, and the drug loading capacity was as high as 32.5%. Therefore, the efficacy of cancer cell killing by photothermal ablation was markedly enhanced by DOX released from the LMHSs. As we expected, the as-made DOX@MoS₂ NPs exhibited excellent photothermo-chemotherapy effect, both