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This work reports the synthesis, characterization, and in vitro release studies of pH- and temperature-sensitive Fe3O4-SiO2-poly(NVCL-co-MAA) nanocomposite. Fe3O4 nanoparticles were prepared by chemical coprecipitation, coated with SiO2 by the Stöber method, and functionalized with vinyl groups. The copolymer poly(N-vinylcaprolactam-co-methacrylic acid) (poly(NVCL-co-MAA)) was grafted onto the functionalized Fe3O4-SiO2 nanoparticles by free radical polymerization. XRD, FTIR, TGA, VSM, and TEM techniques were performed to characterize the nanocomposite. The release behavior of Doxorubicin (DOX) loaded in the nanocomposite at pH 5.8 and 7.4, and two temperatures, 25 and 37 °C, was studied. According to the release studies, approximately 55% of DOX is released in 72 h at pH 7.4, regardless of temperature. At pH 5.8, 78% of DOX was released in 48 h at 25 °C, and when increasing the temperature to 37 °C, more than 95 % of DOX was released in 24 h. The DOX release data treated with Zero-order, first-order, Higuchi, and Korsmeyer–Peppas models showed that Higuchi’s model best fits the data, indicating that the DOX is released by diffusion. The findings suggest that the synthesized nanocomposite may be useful as a DOX carrier in biomedical applications.