Articles written in Bulletin of Materials Science

    • One-pot synthesis of CaAl-layered double hydroxide–methotrexate nanohybrid for anticancer application


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      One-pot (co-precipitation) synthesis route was employed for the first time to synthesize pristine CaAl-layereddouble hydroxide (LDH) and in-situ intercalation of the anticancer drug methotrexate (MTX) to prepare CaAl-LDH–MTXnanohybrid. An increase in the interplanar spacing of the (003) plane from 8.6 $\AA$ in pristine CaAl-LDH bilayered structureto 18.26 $\AA$ in CaAl-LDH–MTX nanohybrid indicated successful intercalation of anionic MTX into the interlayer space ofCaAl-LDH. This was supported by the transmission electron micrographs, which showed an increase in average interlayerspacing from 8.7 $\AA$ in pristine LDH to 18.31 $\AA$ in LDH–MTX nanohybrid. Particle size and morphology analysis of pristineCaAl-LDH and LDH–MTX nanohybrid using both dynamic light scattering (DLS) technique and transmission electronmicroscopy (TEM) indicated a decrease in average particle size in LDH–MTX nanohybrid as compared with that of pristineLDH. Thermogravimetric analyses (TGA) revealed an enhancement in decomposition temperature of MTX bound to CaAl-LDH nanohybrid to 380$^{\circ}$C as compared with 290$^{\circ}$C in pure MTX molecule, indicating enhanced thermal stability, which supports stable electrostatic interaction of MTX within the interlayer position of LDH. CHN (carbon hydrogen nitrogen) analysis revealed nearly 49 wt% of MTX loading into CaAl-LDH, which closely matched with the result obtained from TGA of the nanohybrid. Cumulative release of MTX from CaAl-LDH–MTX in phosphate buffer solution showed a non-lineardependence with incubation time. Release mechanism of MTX from LDH–MTX nanohybrid was governed by diffusionmechanism at physiological pH of 7.4. The in vitro cytotoxicity study of LDH–MTX nanohybrid using MG-63 humanosteosarcoma cell line indicated enhanced inhibition of the cancer cell proliferation compared with the MTX drug alone.

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