To understand the abilities of Ca-alginate microcapsules and their specific applications in different fields, it is necessary to determine the physicochemical and structural properties of those formulated microcapsules. In this work, we aimed to study the effect of alginate concentration in the improvement of the encapsulation efficiency (EE) and on the release of phenolic and flavonoid substances. The relationship between the structure of the encapsulated bioactive substance and Ca-alginate network and their effect on the EE and release kinetics have been investigated. The incorporation, structure, morphology, and phase properties of all elaborated materials were characterized by UV-spectroscopy, Fourier transform infrared (ATR-FTIR), scanning electron microscope (SEM), and X-ray diffraction (DRX). The results indicate that increasing the polymer concentration increases the EE and decreases the loading capacity (LC), whereas the effect of alginate polymer concentration on the release was not observed. The release study of bioactive substances showed that the release kinetics is relatively dependent on the structure and the physicochemical characteristics of the bioactive substance, which became clear when the encapsulated compounds were released from the core of calcium alginate microcapsules. Thus, it could be concluded that the pores size of the Ca-alginate network is smaller than the volume of the crocin molecule (2794.926ų) and higher than the volume of the gallic acid molecule (527.659ų). For the same microcapsules system, the release mechanism is affected by the structure and physicochemical properties of the encapsulated molecules.

The foremost objective of this work is to assess the microcapsules composition (polymer-based and polymer/clay-based) effect, on the release of rosemary essential oil into w/o medium and evaluate their antioxidant activity. Calcium alginate (CA) and calcium alginate/montmorillonite hybrid (CA-MTN) microcapsules were developed following an ionotropic crosslinking gelation and were used as host materials for the encapsulation of rosemary essential oil. The unloaded/loaded CA and hybrid CA-MTN microcapsules were characterized by Fourier transform infra-red (FT-ATR) spectroscopy, thermal analysis (TGA), scanning electron microscopy (SEM) and DPPH assay. The evaluation of the microcapsule’s physicochemical properties has shown that the clay filling with montmorillonite improved the microcapsule’s properties. The encapsulation efficiency improved significantly in hybrid CA-MTN microcapsules and exhibited higher values ranging from 81 for CA to 83% for hybrid CA-MTN and a loading capacity of 71 for CA and 73% for hybrid CA-MTN, owing to the large adsorption capacity of the sodic clay. Moreover, the hybrid CA-MTN microcapsules showed a time-extended release of rosemary essential oil compared to CA microcapsules. Finally, the DPPH assay displayed a higher reduction of free radicals in hybrid CA-MNT-REO (12.8%) than CA-REO (10%) loaded microcapsules. These results proved that the clay–alginate combination provides microcapsules with enhanced properties compared to the polymer-based microcapsules.