Abstract: Traditional chemical fumigants have problems such as environmental pollution, increased pest resistance, and potential threats to human health. Therefore, developing green, efficient, and long-lasting fumigants is a critical measure to ensure the quality of postharvest grains. In this study, the fumigation activity of two plant-derived molecules, 1-octen-3-ol (1-Oc) and linalool (Li) against Sitophilus zeamais was investigated, and a sustained-release system based on Hollow Mesoporous Silica Nanoparticles (HMS) to prolong its insecticidal effect and reduce loss by volatilization was fabricated. It was showed that 1-octen-3-ol and linalool had obvious fumigation activity, and the LC₅₀ of 1-octen-3-ol and linalool at 96 h was 1.51 and 2.98 g/m³, respectively. The synergistic study showed that the combination of 1-octen-3-ol and linalool at the mass ratio of 6: 4 had obvious synergistic effect. The LC50 value of fumigation at 24 h was 2.85 g/m³, and the CTC value was 124.99. In order to improve the shelf life of two small molecules in practical application, three nanoparticles, 1-Oc@HMS, Li@HMS and 1-Oc&Li@HMS were successfully prepared using hollow mesoporous silica as carriers. These three nanoparticles were all hollow spherical with uniform size, and the drug loading rates of 1-Oc@HMS and Li@HMS were 46.25% and 48.19%, respectively, and the drug loading rates of 1-octen-3-ol and linalool in 1-Oc&Li@HMS were 58.00% and 40.00%, respectively. The slow-release performance test showed that under the simulated storage environment, the three kinds of nanoparticles had stable slow-release ability and could slowly release the active ingredients. The cumulative release rates of 1-Oc@HMS, Li@HMS and 1-Oc&Li@HMS reached 27.20 %, 41.87 % and (38.23%, 30.02%) at 9 d, respectively. The fumigation activity and duration of 1-Oc@HMS, Li@HMS and 1-Oc&Li@HMS on Sitophilus zeamais were significantly increased, and the fumigation LC₅₀ at 72 h was 2.94, 10.04 and 2.26 g/m³, respectively. Therefore, the sustained-release system can significantly prolong the volatilization time of 1-octen-3-ol and linalool, improve their persistence in the storage environment, and maintain the high insecticidal activity against Sitophilus zeamais. This study provided a theoretical basis and technical support for the development of new green fumigants, which is expected to play an important role in storage pest control.