Stimuli-responsive biocompatible nanocarriers are very promising for controlled drug release. Here, wereport redox- and temperature-responsive biocompatible nanocapsules prepared by growinga temperature-responsive biocompatible shell from 3-(trimethoxysilyl)propyl methacrylate-modifiedsilica nanoparticles (SiO2-MPS) via precipitation polymerization, cross-linking the shell withbioreducible chemical linkages, and subsequently removing the silica core by hydrofluoric acid etching.The produced nanocapsules are redox- and temperature-responsive. TEM, FT-IR, TGA, and XPSwere used to characterize the nanocapsules. Dynamic light scattering (DLS) was performed todemonstrate the bioreducible and temperature-responsive properties of the nanocapsules. The lowercritical solution temperature (LCST) of the nanocapsules can be tuned precisely. Fluoresceinisothiocyanate (FITC) was encapsulated into the nanocapsules and used as a model drug molecule todemonstrate the controlled release behavior under external stimuli.