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Based on orthogonal test design, the factors influencing the synthesis of methotrexate intercalated magnesium–aluminum layered double hydroxides (MTX/LDHs for short) by ion-exchange method, such as weight ratio of pristine LDHs to MTX ( R for short), exchange temperature, time and pH value were investigated. Of the four controllable independent variables, R had the strongest effect on the crystallinity and the drug-loading capacity and the optimum synthesis conditions considered from the crystallinity and the drug-loading capacity both pointed to the same values, i.e., R =2:1, pH=9.5, temperature of 80 °C and exchange time of 3 day. The XRD diffractions indicated that high MTX content was in favor of the formation of intercalated hybrids, while low content lead to the failure of it. TEM photos indicated that the intercalated hybrids all exhibited aggregated hexagonal plates. In order to improve the morphology, two different states of pristine LDHs, i.e., powder and colloid, were chosen to prepare MTX/LDHs hybrids and the results indicated that colloid state of pristine was advantageous to obtain regular particles. The study also revealed that the properties of hybrids obtained at optimum conditions by ion-exchange were superior to that obtained from standard methods, such as co-precipitation method. [ABSTRACT FROM AUTHOR]

In this paper, the intercalation of methotrexatum (MTX) into layered double hydroxides (LDHs) via an exfoliation-reassembly process was reported and the resulting hybrids were then characterized by X-ray diffraction (XRD) patterns, Fourier transform infrared (FTIR) spectroscopy and atomic force microscopy (AFM) patterns etc. In the synthesis procedure, LDHs particles were firstly delaminated into well-dispersed 2D nanosheets in formamide by ultrasonic treatment at room temperature, and then the resulting LDH nanosheets were reassembled in MTX solution to form MTX intercalated LDH (MTX/LDHs) hybrids. AFM images showed that during the exfoliation process a large part of LDHs particles were delaminated into single and double brucite layers. XRD patterns and FTIR investigations manifested the successful intercalation of MTX anions into LDHs interlayers for the final samples. It was also found out that the drug-loading capacity of the hybrids increased with the concentrations of MTX solutions, while the morphology became even aggregated. At last, the cell cytotoxicity of the hybrids was estimated by MTT assays on the human lung cancer cells (A549), and the results stated that MTX/LDHs hybrids had effective suppress role on the proliferation of cancer cells. [ABSTRACT FROM AUTHOR]