The folic acid (FA) and doxorubicin (DOX) have been doped into the g‐C3N4/MoS2 incorporated‐chitosan/ethyl cellulose (EC) core‐shell nanofibers for targeted delivery of FA and DOX against HeLa and MCF‐7 cell lines. The g‐C3N4/MoS2 nanosheets and core‐shell nanofibers were characterized using Fourier transform infrared spectroscopy, X‐ray diffraction, scanning electron microscopy, transmission electron microscopy, and UV–Vis tests. The drug loading factor, the degradation rate, and the DOX and FA release behavior from core‐shell nanofibers have been investigated. The pharmacokinetic results revealed the linear release with non‐Fickian diffusion of the both anticancer drugs from nanofibers during 7 days. The DAPI staining and MTT assays of the nanofibers immersed in MCF‐7 and HeLa cell lines were studied to determine the potential of DOX and FA doped‐core‐shell nanofibrous matrix for MCF‐7 and HeLa cells death in vitro. The maximum MCF‐7 and HeLa cells death percentages were found to be 89 and 85%, respectively, using EC/chitosan/g‐C3N4/MoS2/DOX/FA core‐shell nanofibers after 7 days. The high activity of g‐C3N4/MoS2/DOX/FA loaded‐core‐shell nanofibers for studied cancer cells killing was achieved.
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