Fabrication of nanostructured mesoporous starch encapsulating soy-derived phytoestrogen (genistein) by well-tuned solvent exchange method

The present research was concerned with preparation of mesoporous starch (MPS) as a carrier for genistein, a model of poorly water-soluble phytoestrogen isoflavone; and exploration of the impact of different fabrication parameters on structural and loading properties. MPS is considered as a highly porous biomaterial which typically possesses nanometer-sized porous microstructure and low density, providing a large effective specific surface area (SSA) and hydrophilic surface to improve solubility, stability and bioavailability of poorly water-soluble active agents. To fabricate MPS, various concentrations (8-14% w/v) of starch from different sources (corn, potato and tapioca) was used for gel formation and the successive solvent exchange process was performed with use of various ethanol concentrations (40-70% v/v), which were then dried by different techniques (rotary vacuum evaporation, microwave and freeze drying). MPS quality attributes such as SSA, total porous volume, BJH pore diameter and swelling ratio were determined and effects of the fabrication parameters were investigated using L9-Taguchi orthogonal array design. The results indicate that second order polynomial regression models were well fitted for all response variables. Interestingly, the starch components greatly influenced physical properties of MPS. Also, the drying type and ethanol concentration altered significantly the model equations. The overall best fabrication condition (14% corn starch, 100% ethanol concentration in aging step and rotary vacuum drying) resulted in favorable MPS preparation with mean size of 105.4 nm and unimodal distribution. In the next step, genistein was encapsulated in MPS microstructure at different ratios, resulting in high loading capacity and efficiency (44.71% and 79.9%, respectively) at 1:1 weight ratio. Equilibrium adsorption isotherm of genistein was evaluated also by four different kinetics models including Langmuir, Freundlich, Dubinin-Radushkevich, and Temkin isotherms. The experimental data were found to be fitted well to the Langmuir model (R² = 0.989). According to the electron microscopy and XRD analysis, the degree of genistein crystallinity lowered remarkably after the impregnation in to MPS, indicating improved solubility. In-vitro release profile of genistein from MPS in the simulated gastrointestinal buffer solutions (pH 1.2 and 6.8) demonstrated that incorporating genistein into the MPS enhanced the dissolution rate compared with genistein powder. Release kinetic data were fitted to the Higuchi model (R² = 0.98), indicating diffusion-controlled release mechanism. Altogether, well-tuned MPS fabrication method can be utilized for an efficient encapsulation and dissolution enhancement of poorly soluble phytochemicals, such as genistein.

Keywords: Encapsulation; Genistein; Polysaccharide aerogel; Poorly water-soluble; Porous materials; Starch.