摘要In situ and real-time monitoring of responsive drug release is critical for the assessment of phar-macodynamics in chemotherapy.In this study,a novel pH-responsive nanosystem is proposed for real-time monitoring of drug release and chemo-phototherapy by surface-enhanced Raman spectroscopy(SERS).The Fe3O4@Au@Ag nanoparticles(NPs)deposited graphene oxide(GO)nanocomposites with a high SERS ac-tivity and stability are synthesized and labeled with a Raman reporter 4-mercaptophenylboronic acid(4-MPBA)to form SERS probes(GO-Fe3O4@Au@Ag-MPBA).Furthermore,doxorubicin(DOX)is attached to SERS probes through a pH-responsive linker boronic ester(GO-Fe3O4@Au@Ag-MPBA-DOX),accom-panying the 4-MPBA signal change in SERS.After the entry into tumor,the breakage of boronic ester in the acidic environment gives rise to the release of DOX and the recovery of 4-MPBA SERS signal.Thus,the DOX dynamic release can be monitored by the real-time changes of 4-MPBA SERS spectra.Additionally,the strong T2 magnetic resonance(MR)signal and NIR photothermal transduction efficiency of the nano-composites make it available for MR imaging and photothermal therapy(PTT).Altogether,this GO-Fe3O4@Au@Ag-MPBA-DOX can simultaneously fulfill the synergistic combination of cancer cell target-ing,pH-sensitive drug release,SERS-traceable detection and MR imaging,endowing it great potential for SERS/MR imaging-guided efficient chemo-phototherapy on cancer treatment.