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This work evaluates cationic intercalation of Capecitabine (Xeloda), an antineoplastic agent in interlayer gallery of Na + -MMT, which was further compounded with Poly ( L -Lactide) to form microcomposite spheres, for oral chemotherapy of breast cancer. The XRD, TGA, SEM, TEM and FT-IR analysis indicated the CAP intercalated in interlayer of MMT and stabilized in the longitudinal monolayer mode by electrostatic interface. No significant alteration in fundamental active properties of CAP was found in the MMT efficacy and data from in vitro study showed controlled drug release pattern >72 h. The efficacy of CAP-MMT hybrid/MPs was also confirmed on Human neuroblastoma cell line (IMR32) by in vitro cell culture experiments evaluating cell cytotoxic and oxidative stress marker indices which showed that intercalated drug and MPs, were as effective as pristine drug. In vivo pharmacokinetics of CAP-MMT hybrids in rats was examined and plasma CAP levels were evaluated. Our findings suggest that CAP-MMT hybrids and MPs can be of considerable value in chemotherapy of malignant neoplastic disease with reduced side effects and clearly demonstrated that MMT not only plays a role as a delivery matrix for drug but also facilitates significant increase in the delivery proficiency.