Optimization of microwave-assisted synthesis of cyclodextrin nanosponges using response surface methodology

Abstract

The reaction of polymerization of cyclodextrins with suitable polyfunctional agents leads to highly cross linked porous structures, referred to as cyclodextrin nanosponges. The conventional heating approach for the synthesis of nanosponges can lead to nonuniform reaction conditions caused by sharp thermal gradients in the bulk solution. In this work, we present a facile method for the synthesis of cyclodextrin nanosponges by microwave irradiation with significant reduction in reaction time. Response surface methodology and Box–Behnken design were used for the optimization of the process parameters including microwave power level (A), reaction time (B) and stirring speed (C). Two dependent variables practical yield and particle size were measured as responses. Mathematical equations and response surface plots were used to relate the dependent variables with independent variables. The optimization model predicted a yield of 96.5287 % and particle size of about 152.355 nm with A, B and C levels of 508.22, 83.55 and 1,471.55 respectively. The observed responses of the optimized process were in close agreement with the predicted values. Three confirmation batches of cyclodextrin nanosponges were synthesized under optimized conditions. The Fourier transformed infrared spectra of nanosponges showed a characteristic peak of the carbonate group at around 1,750 cm⁻¹ which confirms the formation of nanosponges. TGA revealed the stability of obtained nanosponges up to 325 °C. The nanosponges obtained by microwave irradiation exhibited a higher degree of crystallinity. Dimension of the crystal lattice was found to be equal to 0.70 nm. TEM image confirmed the spherical shape and the particle size range of about 153 nm. Compared to conventional heating method, microwave method resulted in four folds reduction in reaction time and provided with particles of homogeneous size distribution and uniform crystallinity.