Mesoporous silica nanoparticles (MSNs) are highly porous carriers used in drug and gene delivery research for biomedical applications due to their high surface area, narrow particle size distribution, and low toxicity. Incorporating disulfide (SS) bonds into the walls of MSNs (MSN-SSs) offers a dual pathway for drug release due to the pore delivery and collapsing porous structure after cellular engulfment. This study explores the effect of embedding disulfide bonds into MSNs through various structural and biological characterization methods. Raman spectroscopy is employed to detect the SS bonds, SEM and TEM for morphology analyses, and a BET analysis to determine the required amount of SSs for achieving the largest surface area. The MSN-SSs are further loaded with doxorubicin, an anticancer drug, to assess drug release behavior under various pH conditions. The MSN-SS system demonstrated an efficient pH-responsive drug release, with over 65% of doxorubicin released under acidic conditions and over 15% released under neutral conditions. Cleaving the SS bonds using dithiothreitol increased the release to 94% in acidic conditions and 46% in neutral conditions. Biocompatibility studies were conducted using cancer cells to validate the engulfment of the nanoparticle. These results demonstrate that MSN-SS is a feasible nanocarrier for controlled-release drug delivery.