The integration of drugs with nanomaterials have received significant interest in the efficient drug delivery systems. Conventional treatments with therapeutically active drugs may cause undesired side effects and, thus, novel strategies to perform these treatments with a combinatorial approach of therapeutic modalities are required. In this study) polymethacrylic acid coated gold nanoparticles (AuNP-PMAA), which were synthesized with reversible addition fragmentation chain transfer (RAFT) polymerization, were combined with doxorubicin (DOX) as a model anticancer drug by creating a pH-sensitive hydrazone linkage in the presence of cysteine (Cys) and cross linker. Drug-AuNP conjugates were characterized via spectrofluorimetry, dynamic light scattering and zeta potential, measurements as well as X-ray photoelectron spectroscopy. The particle size of AuNP-PMAA and AuNP-PMAA-Cys-DOX conjugate were calculated as found as 104 and 147 nm, respectively:. Further experiments with different pH conditions (pH 5.3 and 7.4) also showed that AuNP-PMAA-Cys-DOX conjugate could release the DOX in a pH-sensitive way. Finally, cell culture applications with human cervix adenocarcinoma cell line (HeLa cells) demonstrated effective therapeutic impact of the final conjugate for-both chemotherapy and radiation therapy by comparing free DOX and AuNP-PMAA independently. Moreover, cell imaging study was also an evidence that AuNP-PMAA-Cys-DOX could be a beneficial candidate as a diagnostic agent.